A ramie degumming method combining pretreatment with composite enzymes and its application

Abstract

The invention discloses a ramie degumming method and application of a pretreatment combined with a composite enzyme, and relates to the field of ramie fiber degumming. Before enzymatic degumming of the ramie fiber, the invention first mechanically rolls and boils the ramie fiber, and then performs pretreatment degumming. Borax decomposed by sodium perborate makes the inside of the fiber loose, and degrades the hemicellulose and lignin components of the ramie fiber, destroys the colloid combination, opens the inner wall supported by pectin, and causes the hemicellulose and lignin components to fall off and be removed. The hydrogen peroxide decomposed by sodium perborate in the pretreatment agent at high temperature decolorizes the pigment in the wood cellulose, bleaches the ramie, and can save the subsequent bleaching process for ramie degumming. At the same time, after oxidative degumming, the internal molecules of the ramie fiber are arranged loosely, and the aperture channels are opened, which increases the action sites for the enzyme molecules in the subsequent composite enzyme treatment and improves the reaction efficiency.

Description

Technical Field

[0001] The present invention belongs to the technical field of ramie fiber degumming process methods, and particularly relates to a ramie degumming method combining pretreatment with composite enzymes and its application. Background Art

[0002] Ramie fiber is a kind of green fiber. Ramie contains elements such as dindine, pyrimidine, and purine, which have inhibitory effects on Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, etc. to varying degrees. There are grooved cavities in the middle of its fibers, the tube walls are porous, and they are slender, tough, light in texture, and fast in moisture absorption and dissipation. Therefore, its air permeability is about three times higher than that of cotton fiber. At the same time, ramie fiber has good wearing and service performance, is an excellent textile raw material, and is recognized as the "king of natural fibers". However, ramie contains a large amount of gum, and how to efficiently and greenly remove the gum is the primary problem to be solved currently.

[0003] In the degumming process of ramie, chemical degumming and biological degumming are more commonly used. Chemical degumming achieves the purpose of degumming through acid dipping, alkali liquor boiling, and chlorine bleaching. However, the acid dipping process has strict requirements. If not controlled properly, it will affect the mechanical strength of the raw ramie fiber, and the acid liquor has strong corrosiveness to equipment; the high-temperature boiling process has high water and energy consumption, the COD value in the degumming waste liquid is high, and the wastewater treatment is difficult; chlorine bleaching has a great impact on the environment. Biological degumming includes microbial degumming and enzyme degumming. Among them, enzyme degumming directly uses degumming enzyme preparations or enzymes purified by degumming strains to act on ramie, and uses the biological activity of the enzymes to degrade the gum complex wrapped outside the ramie fiber, so that the fibers are separated. However, the disadvantage of enzyme degumming is that the production cost, storage cost, and selling price are relatively high. Therefore, improving the production efficiency of enzyme degumming is an urgent problem to be solved. Summary of the Invention

[0004] The first object of the present invention is to provide a pretreatment method for oxidative degumming, which can well remove pectin, hemicellulose, and lignin on the raw ramie phloem, and achieve the bleaching effect while removing impurities, thus saving a bleaching process;

[0005] The second object of the present invention is to provide a biological enzyme. Utilizing the characteristics of the enzyme's specific, efficient, and mild conditions, through the synergistic treatment of different components of the enzyme system, pectin and hemicellulose impurities can be removed respectively, reducing the damage to cellulose during the degumming process, making the ramie fiber thinner and softer. After the degummed ramie fiber is spun into linen, the amount of surface fluff is reduced, and the itching sensation after wearing is reduced. Moreover, compared with the traditional chemical degumming method, the process combining the pretreatment of the present invention and enzyme degumming has a low salt concentration, low COD value, and high whiteness in the waste liquid.

[0006] To achieve the first invention object, the ramie is subjected to oxidative pretreatment with a pretreatment agent, which can effectively remove some pectin, lignin and hemicellulose impurities, degrade macromolecular groups into small molecules soluble in water, and introduce surface functional groups such as aldehyde and carboxyl groups. The fineness of the pretreated ramie fiber is better, the water absorption performance is also improved, and at the same time, the bleaching effect is achieved, reducing the damage to equipment, avoiding the bleaching process of sodium hypochlorite in traditional degumming, and the degumming wastewater is easy to treat, thereby reducing the raw material consumption and wastewater discharge;

[0007] To achieve the second invention object, the pretreatment and bio-enzyme treatment are combined. After the pretreatment preliminarily degrades most of the lignin and part of the pectin and hemicellulose, and then through the specific and efficient characteristics of the enzyme, the remaining impurities are further removed. At the same time, the oxidative pretreatment makes the molecular arrangement inside the ramie loose and the pore channels open, increasing the action sites for pectinase and xylanase molecules in the subsequent combined enzyme treatment and improving the reaction efficiency.

[0008] The present invention provides a ramie degumming method combining pretreatment with combined enzymes, comprising the following steps:

[0009] Step 1: Take ramie fibers, comb the head and tail of the ramie fibers, and then repeatedly roll the bast fibers of the raw ramie;

[0010] Step 2: Take peroxide, auxiliary degumming agent, complexing agent, activator, penetrant to prepare a reaction solution, adjust the pH of the reaction solution to 8.0 - 11.0 with an alkali solution, add the ramie rolled in Step 1 for cooking, and turn the ramie over during the cooking process to obtain the pretreated ramie;

[0011] Step 3: Wash the ramie pretreated in Step 2, then prepare an ascorbic acid solution, put the washed ramie into the ascorbic acid solution for treatment, and then beat the ramie and wash it again to obtain the ramie treated with the ascorbic acid solution;

[0012] Step 4: Prepare a combined enzyme mixture from pectin lyase, pectin methylesterase, cutinase and arabinase, then add octyldecanol polyoxyethylene ether, disodium ethylenediaminetetraacetate and water to prepare a combined enzyme working solution, and then use an alkali solution to adjust the pH of the combined enzyme working solution to 7.0 - 11.0, and put the ramie treated with the ascorbic acid solution in Step 3 into the combined enzyme working solution for treatment;

[0013] Step 5: Take alkali, sodium cyclamate, sodium tripolyphosphate, penetrant octyldecanol polyoxyethylene ether to prepare a treatment solution, drain the combined enzyme working solution, then add the treatment solution for cooking, and then beat the ramie and wash it, then dehydrate and shake the ramie;

[0014] Step 6: Prepare an oil solution by taking emulsified oil, emulsifier, and water. Place the ramie treated by shaking in step 5 into the oil solution, let it stand for oiling, and finally dehydrate and dry it to obtain degummed ramie.

[0015] Further, the ramie selected in step 1 is the raw ramie of the next year. The raw ramie is rinsed, dried in the sun, or directly dried in the sun and piled up to obtain the yellow non - cyan ramie bast.

[0016] Further, the number of repeated rolling in step 1 is 1 - 5 times, and specifically it can be selected as 3 times.

[0017] Further, the reaction solution in step 2 is an aqueous solution containing 6 - 14 g / L sodium perborate, 0.5 - 2 g / L CT powder, 0.5 - 2 g / L chelating agent DH - 623J, 1 - 3 g / L Ec - KA3IN 1 pretreatment agent, and 0.5 - 2 g / L penetrant octyldecanol polyoxyethylene ether.

[0018] Preferably, further, the reaction solution in step 2 is an aqueous solution containing 8 - 12 g / L sodium perborate, 0.5 - 2 g / L CT powder, 0.5 - 2 g / L chelating agent DH - 623J, 1 - 3 g / L Ec - KA 3IN 1 pretreatment agent, and 0.5 - 2 g / L penetrant octyldecanol polyoxyethylene ether.

[0019] Specifically, the reaction solution in step 2 is an aqueous solution containing 10 g / L sodium perborate, 1 g / L CT powder, 1 g / L chelating agent DH - 623J, 2 g / L Ec - KA 3IN 1 pretreatment agent, and 1 g / L penetrant octyldecanol polyoxyethylene ether.

[0020] Further, the alkali solution in step 2 is 2 g / L caustic soda.

[0021] Further, the pH of the reaction solution in step 2 is adjusted to 8.0 - 11.0, and specifically it can be selected as 11.0.

[0022] Further, the mass - to - volume ratio of ramie and the reaction solution in step 2 is 500 g:(5 - 10) L.

[0023] Specifically, the mass - to - volume ratio of ramie and the reaction solution in step 2 is 500 g:7.5 L.

[0024] Further, the scouring in step 2 is carried out at 95 °C for 180 minutes.

[0025] Further, during the scouring process in step 2, the ramie should be turned over every 30 minutes.

[0026] Further, the concentration of the ascorbic acid solution in step 3 is 1 - 5 g / L, and specifically it can be selected as 3 g / L.

[0027] Furthermore, the liquor ratio of ramie to ascorbic acid solution in step 3 is 1:(8 - 12), and specifically it can be selected as 1:10.

[0028] Furthermore, the treatment condition in step 3 is to treat for 60 minutes under the condition of 100 °C.

[0029] Furthermore, the mass ratio of pectate lyase to pectin methylesterase in the complex enzyme mixture in step 4 is 1:(0.5 - 3), and specifically it can be selected as 1:1.

[0030] Furthermore, the mass ratio of pectate lyase to cutinase in the complex enzyme mixture in step 4 is 1:(0.5 - 3), and specifically it can be selected as 1:2.

[0031] Furthermore, the weight ratio of pectate lyase to arabinase in the complex enzyme mixture in step 4 is 1:(0.5 - 3), and specifically it can be selected as 1:1.

[0032] Furthermore, the mass ratio of the complex enzyme mixture to octyldodecyl polyethylene glycol in step 4 is 25:(5 - 10), and specifically it can be selected as 25:7.5.

[0033] Furthermore, the mass ratio of the complex enzyme mixture to disodium ethylenediaminetetraacetate in step 4 is 25:(10 - 20), and specifically it can be selected as 25:15.

[0034] Furthermore, the mass - volume ratio of the complex enzyme mixture to water in step 4 is 25 g:(10 - 15) L, and specifically it can be selected as 25 g:12.4 L.

[0035] Furthermore, the alkali solution in step 4 is caustic soda with a concentration of 2 g / L.

[0036] Furthermore, the pH of the reaction solution in step 4 is adjusted to 7.0 - 11.0, and specifically it can be selected as 9.0.

[0037] Furthermore, the mass - volume ratio of ramie to the complex enzyme working solution in step 4 is 500 g:(10 - 15) L, and specifically it can be selected as 500 g:12.4 L.

[0038] Furthermore, the treatment condition in step 4 is to keep warm at 40 - 70 °C for 4 - 17 h.

[0039] Preferably, the treatment condition in step 4 is to keep warm at 45 - 65 °C for 8 - 16 h.

[0040] Specifically, the treatment condition in step 4 can be to keep warm at 55 °C for 12 h.

[0041] Furthermore, the treatment liquid in step 5 is an aqueous solution containing 2-6 g / L caustic soda, 1-3 g / L cyclamate, 0.5-2 g / L sodium tripolyphosphate, and 0.5-2 g / L penetrant polyoxyethylene octanol.

[0042] Specifically, the treatment liquid in step 5 is an aqueous solution containing 4 g / L caustic soda, 2 g / L cyclamate, 1 g / L sodium tripolyphosphate, and 1 g / L penetrant polyoxyethylene octanol.

[0043] Furthermore, in step 5, the bath ratio of ramie to the treatment liquid is 1:(10-14), and can be specifically 1:12.

[0044] Furthermore, in step 5, the scouring is performed at 90° C. for 3 hours.

[0045] Furthermore, the oil solution in step 6 is an aqueous solution containing 4-8 g / L JNM-D1 emulsified oil, 0.5-2 g / L hydrogen peroxide, and 4-8 g / L JNM-D2 emulsifier.

[0046] Specifically, the oil solution in step 6 is an aqueous solution containing 6 g / L JNM-D1 emulsified oil, 1 g / L hydrogen peroxide, and 6 g / L JNM-D2 emulsifier.

[0047] Furthermore, in step 6, the bath ratio of ramie to oil solution is 1:(8-12), and can be specifically 1:10.

[0048] Furthermore, in step 6, the oiling is performed at a temperature of 45° C. for 40 minutes.

[0049] The invention relates to application of the method in processing fabrics, fibers and linen.

[0050] Beneficial effects of the present invention:

[0051] (1) The present invention provides a short-process pretreatment method for effective degumming, which solves the defects of the traditional acid-base pretreatment process, which is long and has high wastewater discharge indicators, and achieves high-quality bleaching effect. The blue light whiteness is 70%, which is higher than the national standard for dried hemp. The traditional chlorine-containing bleaching process is omitted, and the degumming operation process is simple, which continues to retain the environmental protection advantages of enzyme degumming.

[0052] (2) The method provided by the present invention overcomes the low efficiency of the single biological enzyme degumming method. The present invention studies the process of ramie degumming using a composite alkaline biological enzyme after oxidation pretreatment. The existence of the pretreatment step makes the arrangement inside the ramie loose and the aperture channel open, so that the ramie fiber is further exposed, thereby increasing the action sites of subsequent pectinase and xylanase molecules and improving the reaction efficiency. The residual glue rate can reach 3.9%. The final dried ramie fiber has a small decrease in breaking strength, and the fiber surface is smooth and soft to the touch. BRIEF DESCRIPTION OF THE DRAWINGS

[0053] Figure 1 The invention discloses a flow chart of a pretreatment method for ramie bio-enzyme degumming.

[0054] Figure 2 It is a scanning electron microscope picture of raw ramie in a pretreatment method of ramie bioenzyme degumming of the present invention.

[0055] Figure 3 The present invention discloses a scanning electron microscope picture of a ramie pretreatment method for bio-enzyme degumming. DETAILED DESCRIPTION

[0056] The technical solutions in the embodiments of the present invention are further described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention. The following embodiments are illustrative rather than restrictive, and the protection scope of the present invention cannot be limited by the following embodiments.

[0057] The methods used in the present invention, unless otherwise specified, are all conventional methods in the art; the reagents used in the present invention, unless otherwise specified, are all conventional reagents in the art.

[0058] Experimental Materials:

[0059] Ramie raw hemp fiber (Dazhu County, Sichuan), sodium hydroxide, hydrogen peroxide, sodium tripolyphosphate, disodium ethylenediaminetetraacetic acid (Sinopharm Chemical Reagent Co., Ltd.), sodium perborate tetrahydrate, cyclamate (Beijing Bailingwei Technology Co., Ltd.), CT powder (Dongguan Hongshun Chemical Co., Ltd.), chelating agent DH-623J (Jinan Xinyue Chemical Co., Ltd.), Ec-KA 3IN 1 pretreatment agent (Dongfang Meijie Molecular Materials Technology Co., Ltd.), ascorbic acid (Jinan Xinjiulong Biotechnology Co., Ltd.), JFC-6 penetrant (Shandong Yousuo Chemical Technology Co., Ltd.), pectin lyase (680U / ml, Sichuan Lvcheng Biotechnology Co., Ltd.), pectin methylesterase (1000U / ml, Xiasheng Biotechnology Co., Ltd.), T.fusca cutinase (300U / ml, Novozymes Biotechnology Co., Ltd.), arabinase (600U / g, Shanghai Jingke Chemical Technology Co., Ltd.), JNM-D1 emulsified oil, JNM-D2 emulsifier (Huzhou Youjia Biotechnology Co., Ltd.).

[0060] Analysis of ramie ingredients content:

[0061] The determination was carried out according to the quantitative analysis method of ramie chemical components in GBT 5889-1986. The results are shown in Table 1.

[0062] Residual glue rate test method:

[0063] Referring to GBT 5889-1986 ramie chemical composition quantitative analysis method, the residual rubber rate of ramie refined and dried ramie after degumming was tested. The residual rubber rate formula of ramie refined and dried ramie is:

[0064] Residual glue rate (%) = (dry weight of sample - dry weight of sample after residual glue extraction) / dry weight of sample × 100%. The measurement results are shown in Table 2.

[0065] Whiteness test method:

[0066] Referring to GBT 5885-1986 ramie fiber whiteness test method, the whiteness of the degummed ramie was tested. The whiteness calculation formula of the degummed ramie is:

[0067] Whiteness (degree) = average whiteness value of the sample / number of times the sample is measured. The measurement results are shown in Table 2;

[0068] Bundle fiber breaking strength test method:

[0069] The test instrument was purchased from Changzhou No. 1 Textile Factory. The cutting length of the test sample was 40 mm, the sample weight was controlled at about 10 mg, the clamping distance of the machine was adjusted to 10 mm, the stretching speed was 300 mm / min, and the calculation formula of the bundle fiber strength was as follows:

[0070] Linear density (dtex) of the tow = mass of the tow / cut length of the tow × 104

[0071] Breaking strength of tow fiber (cN / detx) = breaking strength of the tow / linear density of the tow. The measurement results are shown in Table 2.

[0072] Example 1

[0073] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0074] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the ramie raw bast fiber with a ramie press 3 times;

[0075] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 8 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 9.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 100 minutes at 70 °C. During the reaction process, turn the ramie over every 30 minutes;

[0076] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution, and treat the washed ramie at 100 °C for 60 minutes with a bath ratio of 1:10. After treatment, beat the ramie and then wash it again;

[0077] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:2:1:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 with 2 g / L of caustic soda. Put the ramie washed in Step 3 into the composite enzyme working solution and keep it at 55 °C for 10 h;

[0078] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, then add the treatment solution with a bath ratio of 1:12, and then boil for 3 h at 70 °C. After weak base refining treatment, beat the ramie and wash it, and then use a laboratory centrifuge for dehydration and a vibrating machine for vibrating treatment;

[0079] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10. Its solvent is water, and the component contents are 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie processed in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0080] The composition of the degumming product obtained in Example 1 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 17.5% (the gum content is not the same as the residual gum rate, which is the content of impurity components excluding the cellulose content).

[0081] Example 2

[0082] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0083] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the bast fiber of the raw ramie with a ramie press 3 times;

[0084] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 9 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 9.5 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 120 minutes at 80 °C. During the reaction process, turn the ramie over every 30 minutes;

[0085] Step 3: Wash the ramie pretreated in Step 2, and then prepare a 3 g / L ascorbic acid solution. At a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes, and perform knocking and washing after treatment;

[0086] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 2:1:1:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then use 2 g / L of caustic soda to adjust the pH of the composite enzyme working solution to 9.0. Put the ramie washed in Step 3 into the composite enzyme working solution and incubate at 55 °C for 12 h;

[0087] Step 5: Prepare a treatment solution with a content of 4 g / L caustic soda, 2 g / L sodium cyclamate, 1 g / L sodium tripolyphosphate, and 1 g / L penetrant octyldecanol polyoxyethylene ether. Drain the compound enzyme working solution, then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 80 °C. After weak alkaline refining treatment, beat the ramie and wash it, then dehydrate it using a laboratory centrifuge and perform ramie shaking treatment using a ramie shaking machine;

[0088] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10, with water as the solvent and component contents of 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0089] The composition of the degumming product obtained in Example 2 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 14.3%.

[0090] Example 3

[0091] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0092] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and use a ramie press to repeatedly roll the raw ramie bast fiber 3 times;

[0093] Step 2: Prepare 7.5 L of reaction solution, with water as the solvent and the contents of the other components being 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 10.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 90 °C. During the reaction process, turn the ramie over every 30 minutes;

[0094] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution. At a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes. After treatment, beat the ramie and wash it again;

[0095] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a compound enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a compound enzyme working solution, and then use 2 g / L of caustic soda to adjust the pH of the compound enzyme working solution to 9.0. Put the ramie washed in Step 3 into the compound enzyme working solution and keep it warm at 45 °C for 8 h;

[0096] Step 5: Prepare a treatment solution with a content of 4 g / L caustic soda, 2 g / L sodium cyclamate, 1 g / L sodium tripolyphosphate, and 1 g / L penetrant octyldecanol polyoxyethylene ether. Drain the compound enzyme working solution, then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 100 °C. After weak alkaline refining treatment, perform knocking and washing of ramie, then dehydrate using a bench centrifuge and perform shaking treatment using a shaking machine for ramie;

[0097] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10, with water as the solvent and component contents of 6 g / L JNM-D1 emulsified oil, 1 g / L hydrogen peroxide, and 6 g / L JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0098] The composition of the degumming product obtained in Example 3 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 12.4%.

[0099] Example 4

[0100] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0101] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and use a ramie press to repeatedly roll the raw ramie bast fiber 3 times;

[0102] Step 2: Prepare 7.5 L of reaction solution, with water as the solvent and the contents of the remaining components being 10 g / L sodium perborate, 1 g / L CT powder, 1 g / L chelating agent DH-623J, 2 g / L Ec-KA 3IN 1 pretreatment agent, and 1 g / L penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction process, turn the ramie over every 30 minutes;

[0103] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution. At a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes, perform knocking after treatment and then wash again;

[0104] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a compound enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a compound enzyme working solution, and then use 2 g / L caustic soda to adjust the pH of the compound enzyme working solution to 9.0. Put the ramie washed in Step 3 into the compound enzyme working solution and keep it at 55 °C for 12 h;

[0105] Step 5: Prepare a treatment solution with a content of 4 g / L sodium hydroxide, 2 g / L sodium cyclamate, 1 g / L sodium tripolyphosphate, and 1 g / L penetrant octyldecanol polyoxyethylene ether. Drain the compound enzyme working solution, and then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 90 °C. After weak alkaline refining treatment, perform knocking and washing of ramie, and then dehydrate using a laboratory centrifuge and perform shaking treatment using a shaking machine for ramie;

[0106] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10, with water as the solvent, and the component content being 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0107] The composition of the degumming product obtained in Example 4 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie decreases from 31.5% of the raw ramie to 10.7%.

[0108] Example 5

[0109] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0110] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the raw ramie bast fiber with a ramie press 3 times;

[0111] Step 2: Prepare 7.5 L of reaction solution, with water as the solvent, and the contents of the other components being 12 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 10.5 with 2 g / L of sodium hydroxide, add the ramie rolled in Step 1, and boil for 180 minutes at 100 °C. During the reaction process, turn over the ramie every 30 minutes;

[0112] Step 3: Wash the ramie pretreated in Step 2, and then prepare a 3 g / L ascorbic acid solution. At a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes. After treatment, perform knocking and then washing;

[0113] Step 4: Mix pectate lyase, pectin methylesterase, cutinase and arabinase in a weight ratio of 1:1:1:2 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, and add 12.4 L of water to prepare a composite enzyme working solution. Then adjust the pH of the composite enzyme working solution to 9.0 using 2 g / L of caustic soda. Place the ramie washed in Step 3 into the composite enzyme working solution and incubate at 55 °C for 10 h;

[0114] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 100 °C. After weak alkali refining treatment, perform knocking and washing of the ramie, and then dehydrate using a laboratory centrifuge and shake the ramie using a shaking machine;

[0115] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10, with water as the solvent. The component content is 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0116] The composition of the degumming product obtained in Example 5 is shown in Table 1. As can be seen from Table 1, the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 6.2%.

[0117] Example 6

[0118] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0119] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the ramie raw bast fiber 3 times using a ramie press;

[0120] Step 2: Prepare 7.5 L of a reaction solution, with water as the solvent, and the content of the remaining components being 12 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 using 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 200 minutes at 100 °C. During the reaction process, turn the ramie over every 30 minutes;

[0121] Step 3: Wash the ramie pretreated in Step 2, and then prepare a 3 g / L ascorbic acid solution. At a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes. After treatment, perform knocking and then washing;

[0122] Step 4: Mix pectate lyase, pectin methylesterase, cutinase and arabinase in a weight ratio of 1:2:1:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate. Add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 using 2 g / L of caustic soda. Place the ramie washed in Step 3 into the composite enzyme working solution and incubate at 55 °C for 10 h;

[0123] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 100 °C. After weak alkaline refining treatment, perform knocking and washing of the ramie, and then dehydrate using a laboratory centrifuge and perform shaking treatment using a shaking machine;

[0124] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10, with water as the solvent and component contents of 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0125] The composition of the degumming product obtained in Example 6 is shown in Table 1. As can be seen from Table 1, the gum content of the obtained degummed ramie decreased from 31.5% of the raw ramie to 5.4%.

[0126] Comparative Example 1

[0127] In this comparative example, ramie was degummed without using a composite enzyme.

[0128] Taking the degumming process of 500 g of ramie fiber as an example, the following steps were used for treatment:

[0129] Step 1: Use a ramie press to repeatedly roll the raw ramie bast fiber 3 times;

[0130] Step 2: Prepare 7.5 L of a reaction solution, with water as the solvent and the remaining component contents being 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 using 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 100 °C. During the reaction process, turn the ramie over every 30 minutes;

[0131] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution. With a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes. After treatment, beat the ramie and then wash it again;

[0132] Step 4: Prepare a treatment solution with a content of 4 g / L caustic soda, 2 g / L sodium cyclamate, 1 g / L sodium tripolyphosphate, and 1 g / L penetrant octyldecanol polyoxyethylene ether. Drain the compound enzyme working solution, then add the treatment solution at a bath ratio of 1:12. After that, boil and refine at 100 °C for 3 h. After weak alkali refining treatment, beat and wash the ramie, then dehydrate it using a sample centrifuge and perform shaking treatment using a shaking machine;

[0133] Step 5: Prepare 5 L of emulsified oil with a bath ratio of 1:10. Its solvent is water, and the component content is 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry it to obtain degummed ramie.

[0134] The composition of the degummed product obtained in Comparative Example 1 is shown in Table 1. It can be seen from Table 1 that without using compound enzyme degumming and only pretreating with sodium perborate, the effect of only pretreatment can only reduce the gum content from 31.5% of the raw ramie to 14.7%;

[0135] Comparative Example 2

[0136] In this comparative example, the raw ramie is not pretreated.

[0137] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0138] Step 1: Use a ramie press to repeatedly roll the bast fiber of raw ramie 3 times;

[0139] Step 2: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:2:1:1 to prepare 25 g of a compound enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a compound enzyme working solution, and then adjust the pH of the compound enzyme working solution to 9.0 using 2 g / L of caustic soda. Put the ramie washed in Step 3 into the compound enzyme working solution and keep it warm at 55 °C for 10 h;

[0140] Step 3: Prepare a treatment solution with a content of 4 g / L caustic soda, 2 g / L sodium cyclamate, 1 g / L sodium tripolyphosphate, and 1 g / L penetrant octyldecanol polyoxyethylene ether. Drain the compound enzyme working solution, then add the treatment solution at a bath ratio of 1:12. After that, boil and refine at 100 °C for 3 h. After weak alkali refining treatment, beat and wash the ramie, then dehydrate it using a sample centrifuge and perform shaking treatment using a shaking machine;

[0141] Step 4: prepare 5L of emulsified oil with a bath ratio of 1:10, wherein the solvent is water, and the component contents are 6g / L of JNM-D1 emulsified oil, 1g / L of hydrogen peroxide, and 6g / L of JNM-D2 emulsifier. The ramie treated in step 5 is allowed to stand at 45°C for 40 minutes to be oiled, and finally dehydrated and dried to obtain refined ramie.

[0142] The composition of the degummed product obtained in Comparative Example 2 is shown in Table 1. It can be seen from Table 1 that without the use of sodium perborate pretreatment, the action of the composite enzyme alone can only reduce the gum content from 31.5% of the original hemp to 21.2%.

[0143] Comparative Example 3

[0144] Taking the degumming process of 500g ramie fiber as an example, the following steps are used for processing:

[0145] Step 1: Take 500g of ramie fiber, comb the ramie fiber head and tail, and use a ramie press to repeatedly roll the ramie raw hemp bast fiber 3 times;

[0146] Step 2: prepare 7.5L reaction solution, wherein the solvent is water, and the contents of the other components are 10g / L sodium perborate, 1g / L CT powder, 1g / L chelating agent DH-623J, 2g / L Ec-KA 3IN 1 pretreatment agent, and 1g / L penetrant octanol polyoxyethylene ether, adjust the pH of the reaction solution to 11.0 with 2g / L caustic soda, add the ramie rolled in step 1, and cook at 95°C for 180 minutes. During the reaction, turn the ramie over every 30 minutes;

[0147] Step 3: Wash the ramie pretreated in step 2, prepare 3g / L ascorbic acid solution, treat the washed ramie at 100°C for 60 minutes at a bath ratio of 1:10, beat the ramie and then wash it;

[0148] Step 4: Prepare 25g of cutinase, add 7.5g of penetrant octanol polyoxyethylene ether, 15g of disodium ethylenediaminetetraacetate, and add 12.4L of water to prepare a composite enzyme working solution, and then use 2g / L caustic soda to adjust the pH of the composite enzyme working solution to 9.0, put the ramie washed in step 3 into the composite enzyme working solution, and keep it warm at 55°C for 12h;

[0149] Step 5: Prepare a treatment solution containing 4g / L caustic soda, 2g / L sodium cyclamate, 1g / L sodium tripolyphosphate, and 1g / L penetrant octanol polyoxyethylene ether. Drain the complex enzyme working solution, add the treatment solution at a bath ratio of 1:12, and then boil at 90°C for 3h. After weak alkali refining treatment, wash with water, and then use a medium sample centrifuge to dehydrate and a shaking machine to shake the hemp.

[0150] Step 6: Prepare 5 L of emulsified oil with a bath ratio of 1:10. Its solvent is water, and the component contents are 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry it to obtain degummed ramie.

[0151] The composition of the degummed product obtained in Comparative Example 3 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie decreased from 31.5% of the raw ramie to 19.7%.

[0152] Comparative Example 4

[0153] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0154] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the bast fiber of the raw ramie with a pressing machine 3 times.

[0155] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction, turn the ramie over every 30 minutes.

[0156] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution. With a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes, and after treatment, beat the ramie and then wash it again.

[0157] Step 4: Mix pectin lyase, pectin methylesterase, and arabinase in a weight ratio of 1:1:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 with 2 g / L of caustic soda. Put the ramie washed in Step 3 into the composite enzyme working solution and incubate at 55 °C for 12 h.

[0158] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution with a bath ratio of 1:12. Then boil for 3 h at 90 °C. After weak alkaline refining treatment, beat the ramie and wash it, and then use a bench centrifuge for dehydration and a shaking machine for shaking treatment.

[0159] Step 6: Prepare 5 L of emulsified oil with a bath ratio of 1:10. Its solvent is water, and the component contents are 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie processed in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry it to obtain degummed ramie.

[0160] The composition of the degummed product obtained in Comparative Example 4 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie ranges from 31.5% of the raw ramie to 9.9%.

[0161] Comparative Example 5

[0162] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0163] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the raw ramie bast fiber with a pressing machine 3 times;

[0164] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction process, turn the ramie over every 30 minutes;

[0165] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution, and treat the washed ramie at 100 °C for 60 minutes with a bath ratio of 1:10. After treatment, beat the ramie and then wash it again;

[0166] Step 4: Mix pectin methyl esterase and cutinase in a weight ratio of 1:1 to prepare 25 g of a composite enzyme mixture, add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then use 2 g / L of caustic soda to adjust the pH of the composite enzyme working solution to 9.0. Put the ramie washed in Step 3 into the composite enzyme working solution and keep it at 55 °C for 12 h;

[0167] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution with a bath ratio of 1:12. Then boil for 3 h at 90 °C. After weak base refining treatment, beat and wash the ramie, and then dehydrate it with a laboratory centrifuge and shake it with a shaking machine;

[0168] Step 6: Prepare 5 L of emulsified oil with a bath ratio of 1:10. Its solvent is water, and the component contents are 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0169] The composition of the degummed product obtained in Comparative Example 5 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 17.5%.

[0170] Comparative Example 6

[0171] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0172] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and use a ramie press to repeatedly roll the bast fiber of the raw ramie 3 times.

[0173] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction, turn the ramie over every 30 minutes.

[0174] Step 3: Wash the ramie pretreated in Step 2, and then prepare a 3 g / L ascorbic acid solution. With a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes, and then beat the ramie and wash it again.

[0175] Step 4: Mix cutinase and arabinase in a weight ratio of 1:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then use 2 g / L of caustic soda to adjust the pH of the composite enzyme working solution to 9.0. Put the ramie washed in Step 3 into the composite enzyme working solution and incubate at 55 °C for 12 h.

[0176] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution with a bath ratio of 1:12. Then boil for 3 h at 90 °C. After weak base refining treatment, beat the ramie and wash it, and then use a bench centrifuge for dehydration and a vibrating machine for vibrating treatment.

[0177] Step 6: Prepare 5 L of emulsified oil with a bath ratio of 1:10. Its solvent is water, and the component contents are 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie processed in Step 5 stand for oiling at 45°C for 40 minutes, and finally dehydrate and dry it to obtain degummed ramie.

[0178] The composition of the degummed product obtained in Comparative Example 6 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 18.1%.

[0179] Comparative Example 7

[0180] This comparative example is the comparative example of Example 4, in which the temperature of the heat preservation treatment in Step 4 is adjusted to 45°C, and other steps remain unchanged.

[0181] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0182] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the bast fiber of the raw ramie with a ramie press 3 times.

[0183] Step 2: Prepare 7.5 L of reaction solution. Its solvent is water, and the contents of the other components are 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95°C. During the reaction process, turn the ramie over every 30 minutes.

[0184] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution. With a bath ratio of 1:10, treat the washed ramie at 100°C for 60 minutes, and then beat the ramie and wash it again after treatment.

[0185] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 with 2 g / L of caustic soda. Put the ramie washed in Step 3 into the composite enzyme working solution and keep it at 45°C for heat preservation treatment for 12 h.

[0186] Step 5: Prepare a treatment solution containing 4g / L caustic soda, 2g / L sodium cyclamate, 1g / L sodium tripolyphosphate, and 1g / L penetrant octanol polyoxyethylene ether. Drain the complex enzyme working solution, add the treatment solution at a bath ratio of 1:12, and then boil at 90°C for 3h. After weak alkali refining treatment, wash with water, and then use a medium sample centrifuge to dehydrate and a shaking machine to shake the hemp.

[0187] Step 6: prepare 5L of emulsified oil with a bath ratio of 1:10, wherein the solvent is water, and the component contents are 6g / L of JNM-D1 emulsified oil, 1g / L of hydrogen peroxide, and 6g / L of JNM-D2 emulsifier. The ramie treated in step 5 is allowed to stand at 45°C for 40 minutes to be oiled, and finally dehydrated and dried to obtain refined ramie.

[0188] The composition of the degummed product obtained in Comparative Example 7 is shown in Table 1. It can be seen from Table 1 that the glue content of the obtained refined hemp is reduced from 31.5% of the original hemp to 13.9%. Compared with Example 4, the residual glue rate is increased to 5.4%, the whiteness is reduced, and the fiber strength is reduced;

[0189] Comparative Example 8

[0190] This comparative example is a comparative example of Example 4, wherein the temperature of the heat preservation treatment in step 4 is adjusted to 65° C., and the other steps remain unchanged.

[0191] Taking the degumming process of 500g ramie fiber as an example, the following steps are used for processing:

[0192] Step 1: Take 500g of ramie fiber, comb the ramie fiber head and tail, and use a ramie press to repeatedly roll the ramie raw hemp bast fiber 3 times;

[0193] Step 2: prepare 7.5L reaction solution, wherein the solvent is water, and the contents of the other components are 10g / L sodium perborate, 1g / L CT powder, 1g / L chelating agent DH-623J, 2g / L Ec-KA 3IN 1 pretreatment agent, and 1g / L penetrant octanol polyoxyethylene ether, adjust the pH of the reaction solution to 11.0 with 2g / L caustic soda, add the ramie rolled in step 1, and cook at 95°C for 180 minutes. During the reaction, turn the ramie over every 30 minutes;

[0194] Step 3: Wash the ramie pretreated in step 2, prepare 3g / L ascorbic acid solution, treat the washed ramie at 100°C for 60 minutes at a bath ratio of 1:10, beat the ramie and then wash it;

[0195] Step 4: Mix pectate lyase, pectin methylesterase, cutinase and arabinase according to a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of the penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate. Add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 using 2 g / L of caustic soda. Put the ramie washed in Step 3 into the composite enzyme working solution and keep it at 65 °C for 12 h;

[0196] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of the penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 90 °C. After weak alkali refining treatment, perform knocking and washing of the ramie, and then use a laboratory centrifuge for dehydration and a shaking machine for shaking treatment;

[0197] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10, with water as the solvent and component contents of 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0198] The composition of the degummed product obtained in Comparative Example 8 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 14.6%. Compared with Example 4, the residual gum rate increases to 5.6%, the whiteness becomes smaller, and the fiber strength decreases;

[0199] Comparative Example 9

[0200] This comparative example is a comparative example of Example 4, in which the holding time in Step 4 is adjusted to 8 h, and other steps remain unchanged.

[0201] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0202] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and use a ramie press to repeatedly roll the raw ramie bast fiber 3 times;

[0203] Step 2: Prepare 7.5 L of a reaction solution, with water as the solvent and the remaining component contents of 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of the penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 using 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction process, turn the ramie over every 30 minutes;

[0204] Step 3: Wash the ramie pre-treated in Step 2, then prepare a 3 g / L ascorbic acid solution. At a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes. After treatment, beat the ramie and then wash it again;

[0205] Step 4: Mix pectate lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of the penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate. Add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 using 2 g / L of caustic soda. Put the ramie washed in Step 3 into the composite enzyme working solution and incubate at 55 °C for 8 h;

[0206] Step 5: Prepare a treatment solution with a content of 4 g / L caustic soda, 2 g / L sodium cyclamate, 1 g / L sodium tripolyphosphate, and 1 g / L penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 90 °C. After weak alkaline refining treatment, beat the ramie and wash it, then dehydrate using a sample centrifuge and shake the ramie using a shaking machine;

[0207] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10. Its solvent is water, and the component content is 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0208] The composition of the degummed product obtained in Comparative Example 9 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie decreased from 31.5% of the raw ramie to 15.1%. Compared with Example 4, the residual gum rate increased to 5.5%, the whiteness decreased, and the fiber strength decreased;

[0209] Comparative Example 10

[0210] This comparative example is a comparative example of Example 4, in which the incubation time in Step 4 is adjusted to 5 h, and other steps remain unchanged.

[0211] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0212] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the raw ramie bast fiber with a ramie press 3 times;

[0213] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction process, turn the ramie over every 30 minutes;

[0214] Step 3: Wash the ramie pretreated in Step 2, and then prepare a 3 g / L ascorbic acid solution. With a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes. After treatment, beat the ramie and then wash it again;

[0215] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then use 2 g / L of caustic soda to adjust the pH of the composite enzyme working solution to 9.0. Put the ramie washed in Step 3 into the composite enzyme working solution and keep it at 55 °C for 5 h;

[0216] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution at a bath ratio of 1:12. Then boil for 3 h at 90 °C. After weak alkali refining treatment, beat the ramie and wash it, and then use a laboratory centrifuge for dehydration and a vibrating machine for vibrating treatment;

[0217] Step 6: Prepare 5 L of emulsified oil with a bath ratio of 1:10, where the solvent is water, and the component contents are 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0218] The composition of the degummed product obtained in Comparative Example 10 is shown in Table 1. As can be seen from Table 1, the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 18.4%. Compared with Example 4, the residual gum rate increases to 6.1%, but the fiber strength decreases;

[0219] Comparative Example 11

[0220] This comparative example is a comparative example of Example 4, in which the holding time of the heat treatment in Step 4 is adjusted to 16 h, and the other steps remain unchanged.

[0221] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0222] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the raw ramie bast fiber with a ramie press 3 times;

[0223] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 10 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction process, turn the ramie over every 30 minutes;

[0224] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution. At a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes. After treatment, beat the ramie and then wash it again;

[0225] Step 4: Mix pectin lyase, pectin methyl esterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then use 2 g / L of caustic soda to adjust the pH of the composite enzyme working solution to 9.0. Put the ramie washed in Step 3 into the composite enzyme working solution and keep it at 55 °C for 16 h;

[0226] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution at a bath ratio of 1:12. Then boil for 3 h at 90 °C. After weak base refining treatment, beat the ramie and wash it, and then use a sample centrifuge for dehydration and a shaking machine for shaking treatment;

[0227] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10, where the solvent is water, and the component content is 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0228] The composition of the degummed product obtained in Comparative Example 11 is shown in Table 1. As can be seen from Table 1, the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 11.7%. Compared with Example 4, the residual gum rate is reduced to 4.0%, but the fiber strength damage increases.

[0229] Comparative Example 12

[0230] This comparative example is the comparative example of Example 4, in which the concentration of sodium perborate in Step 2 is adjusted to 8 g / L, and other steps remain unchanged.

[0231] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0232] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeat rolling the ramie raw bast fiber 3 times with a ramie press.

[0233] Step 2: Prepare 7.5 L of reaction solution, where the solvent is water, and the contents of the other components are 8 g / L of sodium perborate, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction process, turn the ramie over every 30 minutes.

[0234] Step 3: Wash the ramie pretreated in Step 2, then prepare a 3 g / L ascorbic acid solution, and treat the washed ramie at 100 °C for 60 minutes with a bath ratio of 1:10. After treatment, beat the ramie and then wash it again.

[0235] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 with 2 g / L of caustic soda. Put the ramie washed in Step 3 into the composite enzyme working solution and incubate at 55 °C for 12 h.

[0236] Step 5: Prepare a treatment solution with a content of 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the composite enzyme working solution, and then add the treatment solution with a bath ratio of 1:12. Then boil for 3 h at 90 °C. After weak alkaline refining treatment, beat the ramie and wash it, and then dehydrate it with a laboratory centrifuge and shake it with a shaking machine.

[0237] Step 6: Prepare 5 L of emulsified oil with a bath ratio of 1:10, where the solvent is water, and the component content is 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0238] The composition of the degummed product obtained in Comparative Example 12 is shown in Table 1. It can be seen from Table 1 that the glue content of the obtained refined hemp is reduced from 31.5% of the original hemp to 11.8%. Compared with Example 4, the residual glue rate is increased to 4.6%, the whiteness is reduced, and the fiber strength is reduced.

[0239] Comparative Example 13

[0240] This comparative example is a comparative example of Example 4, wherein the concentration of sodium perborate in step 2 is adjusted to 12 g / L, and the other steps remain unchanged.

[0241] Taking the degumming process of 500g ramie fiber as an example, the following steps are used for processing:

[0242] Step 1: Take 500g of ramie fiber, comb the ramie fiber head and tail, and use a ramie press to repeatedly roll the ramie raw hemp bast fiber 3 times;

[0243] Step 2: prepare 7.5L reaction solution, wherein the solvent is water, and the contents of the other components are 12g / L sodium perborate, 1g / L CT powder, 1g / L chelating agent DH-623J, 2g / L Ec-KA 3IN 1 pretreatment agent, and 1g / L penetrant octanol polyoxyethylene ether, adjust the pH of the reaction solution to 11.0 with 2g / L caustic soda, add the ramie rolled in step 1, and cook at 95°C for 180 minutes. During the reaction, turn the ramie over every 30 minutes;

[0244] Step 3: Wash the ramie pretreated in step 2, prepare 3g / L ascorbic acid solution, treat the washed ramie at 100°C for 60 minutes at a bath ratio of 1:10, beat the ramie and then wash it;

[0245] Step 4: Pectin lyase, pectin methylesterase, cutinase and arabinase are mixed in a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture, 7.5 g of a penetrant octanol polyoxyethylene ether, 15 g of disodium ethylenediaminetetraacetate, and 12.4 L of water are added to prepare a composite enzyme working solution, and then the pH of the composite enzyme working solution is adjusted to 9.0 with 2 g / L of caustic soda, and the ramie washed in step 3 is placed in the composite enzyme working solution, and heat-treated at 55° C. for 12 h;

[0246] Step 5: Prepare a treatment solution containing 4g / L caustic soda, 2g / L sodium cyclamate, 1g / L sodium tripolyphosphate, and 1g / L penetrant octanol polyoxyethylene ether. Drain the complex enzyme working solution, add the treatment solution at a bath ratio of 1:12, and then boil at 90°C for 3h. After weak alkali refining treatment, wash with water, and then use a medium sample centrifuge to dehydrate and a shaking machine to shake the hemp.

[0247] Step 6: Prepare 5 L of emulsified oil with a bath ratio of 1:10. Its solvent is water, and the component contents are 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry it to obtain degummed ramie.

[0248] The composition of the degummed product obtained in Comparative Example 13 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie is reduced from 31.5% of the raw ramie to 11.1%, and the residual gum rate is reduced to 3.9%, but the fiber strength damage increases.

[0249] Comparative Example 14

[0250] This comparative example is the comparative example of Example 4, in which sodium perborate in Step 2 is replaced with hydrogen peroxide, and other steps remain unchanged.

[0251] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are used for treatment:

[0252] Step 1: Take 500 g of ramie fiber, comb the head and tail of the ramie fiber, and repeatedly roll the bast fiber of the raw ramie with a pressing machine 3 times;

[0253] Step 2: Prepare 7.5 L of reaction solution. Its solvent is water, and the contents of the other components are 10 g / L of hydrogen peroxide, 1 g / L of CT powder, 1 g / L of chelating agent DH-623J, 2 g / L of Ec-KA 3IN 1 pretreatment agent, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Adjust the pH of the reaction solution to 11.0 with 2 g / L of caustic soda, add the ramie rolled in Step 1, and boil for 180 minutes at 95 °C. During the reaction process, turn the ramie over every 30 minutes;

[0254] Step 3: Wash the ramie pretreated in Step 2, and then prepare a 3 g / L ascorbic acid solution. With a bath ratio of 1:10, treat the washed ramie at 100 °C for 60 minutes, and then beat the ramie and wash it again;

[0255] Step 4: Mix pectin lyase, pectin methylesterase, cutinase, and arabinase in a weight ratio of 1:1:2:1 to prepare 25 g of a composite enzyme mixture. Add 7.5 g of penetrant octyldecanol polyoxyethylene ether and 15 g of disodium ethylenediaminetetraacetate, add 12.4 L of water to prepare a composite enzyme working solution, and then adjust the pH of the composite enzyme working solution to 9.0 with 2 g / L of caustic soda. Put the ramie washed in Step 3 into the composite enzyme working solution and keep it warm at 55 °C for 12 h;

[0256] Step 5: Prepare the treatment solution, which contains 4 g / L of caustic soda, 2 g / L of sodium cyclamate, 1 g / L of sodium tripolyphosphate, and 1 g / L of penetrant octyldecanol polyoxyethylene ether. Drain the compound enzyme working solution, and then add the treatment solution at a bath ratio of 1:12. After that, boil for 3 h at 90 °C. After weak alkali refining treatment, perform knocking and washing of ramie, then dehydrate using a laboratory centrifuge and perform shaking treatment using a ramie shaking machine;

[0257] Step 6: Prepare 5 L of emulsified oil at a bath ratio of 1:10. Its solvent is water, and the component content is 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Let the ramie treated in Step 5 stand for oiling at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0258] The composition of the degummed product obtained in Comparative Example 14 is shown in Table 1. It can be seen from Table 1 that the gum content of the obtained degummed ramie decreased from 31.5% of the raw ramie to 12.8%. After replacing sodium perborate with hydrogen peroxide, the residual gum rate increased, the whiteness decreased, and the fiber breaking strength became lower.

[0259] Comparative Example 15

[0260] Taking the degumming process of 500 g of ramie fiber as an example, the following steps are carried out at a bath ratio of 1:15:

[0261] Step 1: Soak with 2.5 g / L of sulfuric acid at 50 °C for 1 h;

[0262] Step 2: The dosage of sodium hydroxide is 5%, and the dosage of sodium silicate is 4%. Conduct the first boiling for 1.5 h at 100 °C;

[0263] Step 3: The dosage of sodium hydroxide is 15%, the dosage of sodium silicate is 2%, and the dosage of sodium tripolyphosphate is 2%. Conduct the second boiling for 3 h at 100 °C;

[0264] Step 4: Use 2 g / L of sulfuric acid for pickling at room temperature for 5 min;

[0265] Step 5: The dosage of sodium hydroxide is 2%, the dosage of sodium silicate is 3%, and the dosage of octyldecanol polyoxyethylene ether is 1%. Conduct refining for 3 h at 100 °C. After refining, perform knocking, washing, dehydration, and shaking operations on the ramie;

[0266] Step 6: Use 6 g / L of JNM-D1 emulsified oil, 1 g / L of hydrogen peroxide, and 6 g / L of JNM-D2 emulsifier. Treat and oil at 45 °C for 40 minutes, and finally dehydrate and dry to obtain degummed ramie.

[0267] Table 1: Determination of Ramie Composition

[0268]

[0269] Table 2 below presents the analysis results of the residual gum rate, whiteness, and bundle fiber breaking strength of the degummed ramie prepared using Examples 1 to 6 and Comparative Examples 1 to 15 of the present invention.

[0270] Table 2: Test Results of Various Indicators for Examples and Comparative Examples

[0271]

[0272] It can be found from Table 2 that the degummed ramie prepared in Examples 3, 4, 5, and 6 has a low residual gum rate and high whiteness, both higher than the national standard for degummed ramie. Comparing the examples with Comparative Example 3, the breaking strength of the bundle fiber after pretreatment is actually higher than that of the traditional chemical method. However, when the oxidant in the pretreatment agent is excessive and the pH is too high, it will have a certain impact on the breaking strength of the fiber. At this time, the consumption of caustic soda will also increase, which will make the COD index of the wastewater higher. Therefore, the optimal dosage of the oxidant is controlled at 10 g / L. At this time, sodium perborate will decompose hydrogen peroxide under high-temperature alkaline conditions, and the lignin in the ramie fiber will dissolve into small molecules, causing the pigments in the lignin to disappear and increasing the whiteness of the fiber. Comparing the data of Examples 3 and 4 with those of Comparative Examples 1 and 2, it can be found that the effect is average after only using enzymes alone, but the residual gum rate after degumming with composite enzymes will be greatly reduced after using the pretreatment process, and the residual gum rate can be reduced to less than 10% by using the pretreatment process alone.

[0273] In Comparative Examples 3 and 4, the addition of pectin methylesterase reduced the residual gum rate from 8.1% to 5.6%. The effect of simply using pectin methylesterase is very poor, indicating that the addition of pectin methylesterase enables the composite enzymes to play a combined role. In Comparative Examples 5 and 6, pectinase and arabinase were used for composite degumming, and cutinase and arabinase were used in combination, but only the functions of pectate lyase and arabinase were exerted. When the four enzymes are used in combination, the enzyme activity can be mutually improved, and the synergistic effect can be increased, thereby better removing the gum in ramie.

[0274] In the comparison between Comparative Examples 7 - 8 and Example 4, it can be found that after adjusting the enzymolysis time, the overall residual gum rate, whiteness, and bundle fiber breaking strength are all worse than those of Example 4. In the comparison between Comparative Examples 9 - 11 and Example 4, it can be found that as the enzymolysis time prolongs, the whiteness first increases and then decreases, and the bundle fiber breaking strength also first increases and then decreases, indicating that the enzymolysis time needs to be optimized within a certain range. In the comparison between Comparative Examples 12 - 13 and Example 4, it can be found that when the concentration of the oxidant is low, the whiteness of the treated ramie is insufficient, but when the concentration of the oxidant is too high, the breaking strength of the bundle fiber of the treated ramie is poor.

[0275] Using the method of combining the pretreatment agent of the present invention with composite enzyme degumming to degum ramie, the obtained ramie fiber was subjected to electron microscopy scanning, and the results are as Figure 2 and Figure 3 shown. FromFigure 2 and Figure 3 It can be seen that the ramie raw fiber is coated with gum and cannot present a single fiber state. After the ramie raw fiber is processed by the steps of this invention, the gum coating the fiber is completely removed, the fiber surface becomes smooth, and the transverse joints and longitudinal stripes of the fiber can be clearly seen, and single ramie fibers can be separated out.

[0276] This invention has studied the process of degumming ramie with composite alkaline bio-enzymes after pretreatment. The existence of the pretreatment process omits the chlorine bleaching process of the traditional process, and the degumming operation process is simple, and the environmental protection advantages of bio-enzymatic degumming are continuously retained.

[0277] Although this invention has been disclosed above with preferred embodiments, it is not intended to limit this invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of this invention. Various modifications to these embodiments will be obvious to those skilled in the art. The general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of this invention. Therefore, this invention will not be limited to these embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A ramie degumming method using a combination of pretreatment and composite enzymes, characterized in that, it includes the following steps: Step 1: Take ramie fibers, comb the head and tail of the ramie fibers, and then repeatedly roll the bast fibers of the raw ramie; Step 2: Take peroxide, auxiliary degumming agent, complexing agent, activator, penetrant to prepare a reaction solution, adjust the pH of the reaction solution to 8.0 - 11.0 with an alkali solution, add the ramie rolled in Step 1 for cooking, and during the cooking process, turn over the ramie to obtain pretreated ramie; Step 3: Wash the pretreated ramie in Step 2, then prepare an ascorbic acid solution, put the washed ramie into the ascorbic acid solution for treatment, and then perform knocking and washing again to obtain ramie treated with the ascorbic acid solution; Step 4: Prepare a composite enzyme mixture from pectin lyase, pectin methylesterase, cutinase and arabinase, then add polyoxyethylene octyl decyl ether, disodium ethylenediaminetetraacetate and water to prepare a composite enzyme working solution, and then use an alkali solution to adjust the pH of the composite enzyme working solution to 7.0 - 11.0, and put the ramie treated with the ascorbic acid solution in Step 3 into the composite enzyme working solution for treatment; Step 5: Take alkali, sodium cyclamate, sodium tripolyphosphate, penetrant polyoxyethylene octyl decyl ether to prepare a treatment solution, drain the composite enzyme working solution, then add the treatment solution, cook, and then perform knocking and washing, and then dehydrate and shake the ramie; Step 6: Take emulsified oil, emulsifier, water to prepare an oil solution, put the ramie shaken in Step 5 into the oil solution for static oiling, and finally dehydrate and dry to obtain degummed ramie; The reaction solution in Step 2 is an aqueous solution containing 6 - 14 g / L sodium perborate, 0.5 - 2 g / L CT powder, 0.5 - 2 g / L chelating agent DH - 623J, 1 - 3 g / L Ec - KA 3IN 1 pretreatment agent, 0.5 - 2 g / L penetrant polyoxyethylene octyl decyl ether; In the composite enzyme mixture in Step 4, the mass ratio of pectin lyase to pectin methylesterase is 1:(0.5 - 3); in the composite enzyme mixture in Step 4, the mass ratio of pectin lyase to cutinase is 1:(0.5 - 3); in the composite enzyme mixture in Step 4, the weight ratio of pectin lyase to arabinase is 1:(0.5 - 3).

2. The method according to claim 1, characterized in that, in Step 2, the mass - to - volume ratio of ramie to the reaction solution is 500 g:(5 - 10) L.

3. The method according to claim 1, characterized in that, in Step 3, the concentration of the ascorbic acid solution is 1 - 5 g / L; in Step 3, the bath ratio of ramie to the ascorbic acid solution is 1:(8 - 12).

4. The method according to claim 1, characterized in that, in Step 4, the mass ratio of the composite enzyme mixture to polyoxyethylene octyl decyl ether is 25:(5 - 10); in Step 4, the mass ratio of the composite enzyme mixture to disodium ethylenediaminetetraacetate is 25:(10 - 20).

5. The method according to claim 1, characterized in that, in Step 4, the mass - to - volume ratio of the composite enzyme mixture to water is 25 g:(10 - 15) L; in Step 4, the mass - to - volume ratio of ramie to the composite enzyme working solution is 500 g:(10 - 15) L.

6. The method according to claim 1, characterized in that, in step 4, the treatment condition is heat preservation treatment at 40-70 °C for 4-17 h.

7. The method according to claim 1, characterized in that, in step 5, the treatment liquid is an aqueous solution containing 2-6 g / L of caustic soda, 1-3 g / L of sodium cyclamate, 0.5-2 g / L of sodium tripolyphosphate, and 0.5-2 g / L of penetrant octyldecanol polyoxyethylene ether; the bath ratio of ramie to the treatment liquid in step 5 is 1:(10-14).

8. The method according to claim 1, characterized in that, in step 6, the oil solution is an aqueous solution containing 4-8 g / L of JNM-D1 emulsified oil, 0.5-2 g / L of hydrogen peroxide, and 4-8 g / L of JNM-D2 emulsifier; the bath ratio of ramie to the oil solution in step 6 is 1:(8-12).

9. Application of the method according to any one of claims 1-8 in fabric or fiber treatment.

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