A refining agent for improving penetration emulsification and preparation method thereof

Abstract

The present invention belongs to the technical field of fabric dyeing and finishing, and specifically relates to a refining agent for improving penetration emulsification and a preparation method thereof. The refining agent of the present invention selects products such as pine alcohol and rosin amine that can be processed from natural products as raw materials on the basis of the prior art, and the prepared pine alcohol polyoxypropylene polyoxyethylene ether has good wettability and permeability, and the rosin amine polyoxyethylene ether not only has low raw material toxicity and is renewable, but also the rosin amine group as the lipophilic end makes it have excellent emulsification performance and stability, and the propylene glycol polyoxyethylene ether fatty acid ester has excellent wettability, compatibilization and permeability, and can improve the emulsification stability of the refining agent. The refining agent prepared by the blending and compounding of the present invention has excellent permeability, emulsification and dispersion stability, and the preparation process is simple, easy to industrially produce, can effectively remove impurities in the fabric, and the treated fabric has good whiteness, excellent hair effect, small fabric strength loss, and no creases.

Description

Technical Field

[0001] The invention belongs to the technical field of fabric dyeing and finishing, and particularly relates to a scouring agent for improving penetration and emulsification and a preparation method thereof. Background Art

[0002] Cotton is the basic raw material of the textile industry, but it contains natural impurities including pigments, pectin and wax, which lead to poor wettability and permeability of cotton fabrics, and the phenomenon that cotton fabrics tend to turn yellow. Therefore, cotton fabrics need to be pre-treated before printing, dyeing and finishing to achieve the purpose of impurity removal and bleaching. In order to improve the efficiency of cotton fabric pre-treatment and product quality, it is usually necessary to add refining agents to improve the permeability and emulsification dispersibility of cotton fabrics.

[0003] Publication No. CN112813691A discloses a refining agent, which includes a penetrant, an emulsifier and a solvent, wherein the penetrant and the emulsifier are dissolved in the solvent; the chemical formula of the penetrant is:

[0004] The chemical formula of the emulsifier is: Wherein, R1 is a branched alkyl group, and R3 is a straight-chain alkyl group. The scouring agent provided by the patent has good low foaming property, good permeability and emulsification, can effectively remove impurities in fabrics, and the treated fabrics have good whiteness, excellent hair effect, small fabric strength loss, and no creases. However, the scouring agent used in fabric dyeing and finishing in the prior art still needs to improve its composition to solve the technical problems of emulsification, wettability and biodegradability to be improved. Summary of the invention

[0005] The purpose of the present invention is to provide a scouring agent with improved penetration emulsification and a preparation method thereof, which is used to solve the technical problem that the scouring agent used in fabric dyeing and finishing in the prior art still needs to improve its ingredients to solve the emulsification, wettability and biodegradability that need to be improved.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] The invention provides a refining agent for improving penetration emulsification. The refining agent is prepared from the following components in parts by weight: 15 to 20 parts of pine alcohol polyoxypropylene polyoxyethylene ether, 15 to 20 parts of sodium alkyl sulfonate, 10 to 20 parts of rosin amine polyoxyethylene ether, 10 to 20 parts of propylene glycol polyoxyethylene ether fatty acid ester and 20 to 50 parts of deionized water.

[0008] Preferably, the number of polyoxypropylenes in the pineol polyoxypropylene polyoxyethylene ether is between 1 and 3, and the number of polyoxyethylenes is between 15 and 20.

[0009] Preferably, the alkyl carbon chain number of the sodium alkyl sulfonate is between 12 and 18.

[0010] Preferably, the polyoxyethylene number of the rosin amine polyoxyethylene ether is between 15 and 20.

[0011] Preferably, the polyoxyethylene number of the propylene glycol polyoxyethylene ether fatty acid ester is between 4 and 7.

[0012] The present invention also provides a method for preparing a refining agent for improving penetration emulsification, comprising the following steps:

[0013] S1, add pine alcohol polyoxypropylene polyoxyethylene ether, sodium alkyl sulfonate, rosin amine polyoxyethylene ether and propylene glycol polyoxyethylene ether fatty acid ester into a mixing kettle in sequence, and stir at 40-50° C. for 30-50 minutes to obtain a mixed solution;

[0014] S2. Add deionized water into the mixed solution for dilution to obtain a refining agent for improving penetration and emulsification.

[0015] The chemical formula for the synthesis of pineol polyoxypropylene polyoxyethylene ether is as follows:

[0016]

[0017] Preferably, the preparation method of pineol polyoxypropylene polyoxyethylene ether comprises the following steps:

[0018] S11, add terpineol into the reactor, introduce nitrogen to replace the air 3 times, heat to 80-90°C and dehydrate under negative pressure for 0.5-1h, add propylene oxide, heat to 120-140°C and react for 3-4h;

[0019] S12, after the reaction is completed, the temperature is lowered to 70-80°C, and nitrogen is introduced to remove unreacted propylene oxide to obtain a terpineol polyoxypropylene ether intermediate product;

[0020] S13, adding the first catalyst and ethylene oxide to the pinene alcohol polyoxypropylene ether intermediate product, raising the temperature to 120-140° C. for reaction for 3-5 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude product of pinene alcohol polyoxypropylene polyoxyethylene ether;

[0021] S14, neutralizing the crude product of pineol polyoxypropylene polyoxyethylene ether with 10wt% hydrochloric acid to neutrality, and filtering to obtain pineol polyoxypropylene polyoxyethylene ether.

[0022] Preferably, the first catalyst in S13 is one or more combinations of sodium hydroxide, potassium hydroxide and sodium hydride.

[0023] Preferably, the weight parts of each substance used in the preparation process of the pineol polyoxypropylene polyoxyethylene ether are 20 parts of pineol, 8-25 parts of propylene oxide, 0.5-2 parts of the first catalyst and 85-115 parts of ethylene oxide.

[0024] Among them, the synthesis process of rosin amine polyoxyethylene ether involves the following two chemical reactions:

[0025] The chemical formula for the synthesis of rosin amine polyoxyethylene ether is as follows:

[0026]

[0027] The chemical formula for the synthesis of dehydrogenated rosin amine polyoxyethylene ether is as follows:

[0028]

[0029] Preferably, the preparation method of rosin amine polyoxyethylene ether comprises the following steps:

[0030] S21, adding rosin amine compounds into the reaction kettle, introducing nitrogen to replace air 3 times, heating to 80-90°C for negative pressure dehydration for 0.5-1h, adding the first part of ethylene oxide, heating to 120-140°C for reaction for 3-4h;

[0031] S22, after the reaction is completed, the temperature is lowered to 70-80°C, and nitrogen is introduced to remove unreacted ethylene oxide to obtain a rosin amine polyoxyethylene ether intermediate product;

[0032] S23, adding the second catalyst and the second part of ethylene oxide to the rosin amine polyoxyethylene ether intermediate product, raising the temperature to 120-140° C. and aging for 3-5 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude rosin amine polyoxyethylene ether;

[0033] S24, neutralizing the crude rosin amine polyoxyethylene ether with 10 wt % hydrochloric acid until neutral, and filtering to obtain the rosin amine polyoxyethylene ether.

[0034] Preferably, the rosin amine compound in S21 is one or both of rosin amine and dehydrorosin amine.

[0035] Preferably, the second catalyst in S23 is one or more combinations of sodium hydroxide, potassium hydroxide and sodium hydride.

[0036] Preferably, the weight parts of each substance used in the preparation process of the rosin amine polyoxyethylene ether are 20 parts of rosin amine compound, 6-7 parts of the first part of ethylene oxide, 0.5-2 parts of the second catalyst and 40-60 parts of the second part of ethylene oxide.

[0037] Preferably, the preparation method of propylene glycol polyoxyethylene ether fatty acid ester comprises the following steps:

[0038] S31, adding propylene glycol polyoxyethylene ether into a reaction kettle, heating to 50-60° C. under stirring, adding an esterification catalyst and fatty acid, heating to 130-150° C. and reacting for 3-4 hours to obtain a crude product of propylene glycol polyoxyethylene ether fatty acid ester;

[0039] S32, adding a sufficient amount of alkaline solution to the crude product of propylene glycol polyoxyethylene ether fatty acid ester to neutralize it, washing the crude product of propylene glycol polyoxyethylene ether fatty acid ester with a saturated salt solution, and purifying it to obtain propylene glycol polyoxyethylene ether fatty acid ester.

[0040] Preferably, the esterification catalyst in S31 is one or more combinations of p-toluenesulfonic acid, potassium hydroxide and zinc oxide.

[0041] Preferably, the fatty acid in S31 is one or more combinations of lauric acid, myristic acid, palmitic acid and stearic acid.

[0042] Preferably, the alkaline solution in S32 is one or more combinations of sodium bicarbonate solution, potassium bicarbonate solution, sodium hydroxide solution and potassium hydroxide solution.

[0043] Preferably, the saturated salt solution in S32 is one or more combinations of saturated sodium chloride solution, saturated calcium chloride solution and saturated sodium carbonate solution.

[0044] Preferably, the weight parts of each substance used in the preparation process of the propylene glycol polyoxyethylene ether fatty acid ester are 20 parts of propylene glycol polyoxyethylene ether, 0.5-2 parts of esterification catalyst and 20-50 parts of fatty acid.

[0045] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0046] 1. The scouring agent of the present invention uses pine alcohol, rosin amine and other products that can be processed from natural products as raw materials on the basis of the existing technology. The scouring agent prepared by blending and compounding has excellent permeability, emulsification and dispersion stability, and the preparation process is simple and easy to industrially produce. After the scouring agent is applied to fabric dyeing and finishing, it can effectively remove impurities in the fabric, and the treated fabric has good whiteness, excellent hair effect, small fabric strength loss and no creases.

[0047] 2. The pine alcohol polyoxypropylene polyoxyethylene ether of the present invention has a pine alcohol group at the oleophilic end and a polyoxyethylene group at the hydrophilic end, and therefore has good wettability and permeability. The introduced pine alcohol group has low toxicity and good biodegradability. The introduced polyoxypropylene group increases the hydrophobic group, thereby enhancing the lipophilicity of the pine alcohol polyoxypropylene polyoxyethylene ether and improving its emulsification. The polyoxyethylene ether chain is segmented with polyoxypropylene to improve its long chain stability.

[0048] 3. The rosin amine polyoxyethylene ether of the present invention introduces rosin amine groups, which not only makes the raw material low in toxicity and renewable, but also has excellent emulsifying properties and stability due to the rosin amine groups as lipophilic ends.

[0049] 4. The propylene glycol polyoxyethylene ether fatty acid ester of the present invention has good surface activity, can reduce the surface tension of water, has excellent wettability, compatibilization and permeability, and can be used in combination with pine alcohol polyoxypropylene polyoxyethylene ether and rosin amine polyoxyethylene ether to improve the emulsification stability of the refining agent. DETAILED DESCRIPTION

[0050] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0051] Example 1. A refining agent for improving penetration and emulsification in this example is prepared from the following ingredients in parts by weight: 20 parts of pine alcohol polyoxypropylene polyoxyethylene ether, 15 parts of sodium alkyl sulfonate, 10 parts of rosin amine polyoxyethylene ether, 10 parts of propylene glycol polyoxyethylene ether fatty acid ester and 30 parts of deionized water.

[0052] The polyoxypropylene number of the pine alcohol polyoxypropylene polyoxyethylene ether is 1, the polyoxyethylene number is 16, the alkyl carbon chain number of the sodium alkyl sulfonate is 12, the polyoxyethylene number of the rosin amine polyoxyethylene ether is 18, and the polyoxyethylene number of the propylene glycol polyoxyethylene ether fatty acid ester is 4.

[0053] A method for preparing a refining agent for improving penetration emulsification in this embodiment includes the following steps:

[0054] S1, add pine alcohol polyoxypropylene polyoxyethylene ether, sodium alkyl sulfonate, rosin amine polyoxyethylene ether and propylene glycol polyoxyethylene ether fatty acid ester into a mixing kettle in sequence, and stir at 40° C. for 30 minutes to obtain a mixed solution;

[0055] S2. Add deionized water into the mixed solution for dilution to obtain a refining agent for improving penetration and emulsification.

[0056] The preparation method of pinene alcohol polyoxypropylene polyoxyethylene ether of this embodiment comprises the following steps:

[0057] S11, add 20 parts of terpineol into the reactor, introduce nitrogen to replace the air 3 times, heat to 85°C and dehydrate under negative pressure for 1 hour, then add 8 parts of propylene oxide, heat to 130°C and react for 3 hours;

[0058] S12, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted propylene oxide to obtain a terpineol polyoxypropylene ether intermediate product;

[0059] S13, adding 1 part of sodium hydroxide and 92 parts of ethylene oxide to the intermediate product of pinene alcohol polyoxypropylene ether, raising the temperature to 130° C. for reaction for 4 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude product of pinene alcohol polyoxypropylene polyoxyethylene ether;

[0060] S14, neutralizing the crude product of pineol polyoxypropylene polyoxyethylene ether with 10wt% hydrochloric acid to neutrality, and filtering to obtain pineol polyoxypropylene polyoxyethylene ether.

[0061] The preparation method of the rosin amine polyoxyethylene ether of this embodiment comprises the following steps:

[0062] S21, add 20 parts of rosin amine into the reaction kettle, introduce nitrogen to replace the air 3 times, heat to 85°C and dehydrate under negative pressure for 1 hour, then add 6.5 parts of the first part of ethylene oxide, heat to 130°C and react for 3 hours;

[0063] S22, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted ethylene oxide to obtain a rosin amine polyoxyethylene ether intermediate product;

[0064] S23, adding 1 part of sodium hydroxide and 52 parts of the second part of ethylene oxide to the rosin amine polyoxyethylene ether intermediate product, heating to 130° C. and aging for 4 hours, and removing unreacted ethylene oxide in vacuo after cooling to obtain a crude rosin amine polyoxyethylene ether;

[0065] S24, neutralizing the crude rosin amine polyoxyethylene ether with 10 wt % hydrochloric acid until neutral, and filtering to obtain the rosin amine polyoxyethylene ether.

[0066] The preparation method of propylene glycol polyoxyethylene ether fatty acid ester of the present embodiment comprises the following steps:

[0067] S31, adding 20 parts of propylene glycol polyoxyethylene ether with a polyoxyethylene number of 4 into a reaction kettle, heating to 60° C. under stirring, adding 1 part of p-toluenesulfonic acid and 25 parts of lauric acid, and then heating to 140° C. for reaction for 4 hours to obtain a crude product of propylene glycol polyoxyethylene ether fatty acid ester;

[0068] S32, adding a sufficient amount of 10wt% sodium bicarbonate solution to the crude product of propylene glycol polyoxyethylene ether fatty acid ester to neutralize it, washing the crude product of propylene glycol polyoxyethylene ether fatty acid ester with a saturated sodium chloride solution, and purifying to obtain propylene glycol polyoxyethylene ether fatty acid ester.

[0069] Example 2. A refining agent for improving penetration and emulsification in this example is prepared from the following ingredients in parts by weight: 15 parts of pine alcohol polyoxypropylene polyoxyethylene ether, 15 parts of sodium alkyl sulfonate, 10 parts of rosin amine polyoxyethylene ether, 10 parts of propylene glycol polyoxyethylene ether fatty acid ester and 20 parts of deionized water.

[0070] The polyoxypropylene number of the pine alcohol polyoxypropylene polyoxyethylene ether is 2, the polyoxyethylene number is 16, the alkyl carbon chain number of the sodium alkyl sulfonate is 16, the polyoxyethylene number of the rosin amine polyoxyethylene ether is 15, and the polyoxyethylene number of the propylene glycol polyoxyethylene ether fatty acid ester is 5.

[0071] A method for preparing a refining agent for improving penetration emulsification in this embodiment includes the following steps:

[0072] S1, adding pine alcohol polyoxypropylene polyoxyethylene ether, sodium alkyl sulfonate, rosin amine polyoxyethylene ether and propylene glycol polyoxyethylene ether fatty acid ester into a mixing kettle in sequence, stirring at 50° C. for 30 minutes to obtain a mixed solution;

[0073] S2. Add deionized water into the mixed solution for dilution to obtain a refining agent for improving penetration and emulsification.

[0074] The preparation method of pinene alcohol polyoxypropylene polyoxyethylene ether of this embodiment comprises the following steps:

[0075] S11, add 20 parts of terpineol into the reactor, introduce nitrogen to replace the air 3 times, heat to 85°C and dehydrate under negative pressure for 1 hour, then add 15 parts of propylene oxide, heat to 130°C and react for 3 hours;

[0076] S12, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted propylene oxide to obtain a terpineol polyoxypropylene ether intermediate product;

[0077] S13, adding 1 part of potassium hydroxide and 91 parts of ethylene oxide to the intermediate product of pinene alcohol polyoxypropylene ether, raising the temperature to 130° C. for reaction for 4 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude product of pinene alcohol polyoxypropylene polyoxyethylene ether;

[0078] S14, neutralizing the crude product of pineol polyoxypropylene polyoxyethylene ether with 10wt% hydrochloric acid to neutrality, and filtering to obtain pineol polyoxypropylene polyoxyethylene ether.

[0079] The preparation method of the rosin amine polyoxyethylene ether of this embodiment comprises the following steps:

[0080] S21, add 20 parts of rosin amine into the reaction kettle, introduce nitrogen to replace the air 3 times, heat to 80°C and dehydrate under negative pressure for 1 hour, then add 6.5 parts of the first part of ethylene oxide, heat to 130°C and react for 3 hours;

[0081] S22, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted ethylene oxide to obtain a rosin amine polyoxyethylene ether intermediate product;

[0082] S23, adding 1 part of potassium hydroxide and 42 parts of the second part of ethylene oxide to the rosin amine polyoxyethylene ether intermediate product, heating to 130° C. and aging for 4 hours, and removing unreacted ethylene oxide in vacuo after cooling to obtain a crude rosin amine polyoxyethylene ether;

[0083] S24, neutralizing the crude rosin amine polyoxyethylene ether with 10 wt % hydrochloric acid until neutral, and filtering to obtain the rosin amine polyoxyethylene ether.

[0084] The preparation method of propylene glycol polyoxyethylene ether fatty acid ester of the present embodiment comprises the following steps:

[0085] S31, adding 20 parts of propylene glycol polyoxyethylene ether with a polyoxyethylene number of 5 into a reaction kettle, heating to 60° C. under stirring, adding 1 part of p-toluenesulfonic acid and 31 parts of myristic acid, and then heating to 150° C. for reaction for 4 hours to obtain a crude product of propylene glycol polyoxyethylene ether fatty acid ester;

[0086] S32, adding a sufficient amount of 10wt% potassium bicarbonate solution to the crude product of propylene glycol polyoxyethylene ether fatty acid ester to neutralize it, washing the crude product of propylene glycol polyoxyethylene ether fatty acid ester with a saturated potassium carbonate solution, and purifying to obtain propylene glycol polyoxyethylene ether fatty acid ester.

[0087] Example 3, a refining agent for improving penetration and emulsification of this example is prepared from the following ingredients in parts by weight: 15 parts of pine alcohol polyoxypropylene polyoxyethylene ether, 15 parts of sodium alkyl sulfonate, 20 parts of rosin amine polyoxyethylene ether, 20 parts of propylene glycol polyoxyethylene ether fatty acid ester and 50 parts of deionized water.

[0088] The polyoxypropylene number of the pine alcohol polyoxypropylene polyoxyethylene ether is 3, the polyoxyethylene number is 20, the alkyl carbon chain number of the sodium alkyl sulfonate is 18, the polyoxyethylene number of the rosin amine polyoxyethylene ether is 20, and the polyoxyethylene number of the propylene glycol polyoxyethylene ether fatty acid ester is 7.

[0089] A method for preparing a refining agent for improving penetration emulsification in this embodiment includes the following steps:

[0090] S1, add pine alcohol polyoxypropylene polyoxyethylene ether, sodium alkyl sulfonate, rosin amine polyoxyethylene ether and propylene glycol polyoxyethylene ether fatty acid ester into a mixing kettle in sequence, and stir at 50° C. for 50 min to obtain a mixed solution;

[0091] S2. Add deionized water into the mixed solution for dilution to obtain a refining agent for improving penetration and emulsification.

[0092] The preparation method of pinene alcohol polyoxypropylene polyoxyethylene ether of this embodiment comprises the following steps:

[0093] S11, add 20 parts of terpineol into the reactor, introduce nitrogen to replace the air 3 times, heat to 90°C and dehydrate under negative pressure for 1 hour, then add 15 parts of propylene oxide, heat to 130°C and react for 4 hours;

[0094] S12, after the reaction is completed, the temperature is lowered to 70° C., and nitrogen is introduced to remove unreacted propylene oxide to obtain a terpineol polyoxypropylene ether intermediate product;

[0095] S13, adding 2 parts of sodium hydride and 115 parts of ethylene oxide to the intermediate product of pinene alcohol polyoxypropylene ether, raising the temperature to 140° C. for reaction for 4 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude product of pinene alcohol polyoxypropylene polyoxyethylene ether;

[0096] S14, neutralizing the crude product of pineol polyoxypropylene polyoxyethylene ether with 10wt% hydrochloric acid to neutrality, and filtering to obtain pineol polyoxypropylene polyoxyethylene ether.

[0097] The preparation method of the rosin amine polyoxyethylene ether of this embodiment comprises the following steps:

[0098] S21, add 20 parts of rosin amine into the reaction kettle, introduce nitrogen to replace the air 3 times, heat to 80°C and dehydrate under negative pressure for 1 hour, then add 7 parts of the first part of ethylene oxide, heat to 130°C and react for 3 hours;

[0099] S22, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted ethylene oxide to obtain a rosin amine polyoxyethylene ether intermediate product;

[0100] S23, adding 0.5 parts of sodium hydride and 60 parts of the second part of ethylene oxide to the rosin amine polyoxyethylene ether intermediate product, heating to 140° C. and aging for 5 hours, and removing unreacted ethylene oxide in vacuo after cooling to obtain a crude rosin amine polyoxyethylene ether;

[0101] S24, neutralizing the crude rosin amine polyoxyethylene ether with 10 wt % hydrochloric acid until neutral, and filtering to obtain the rosin amine polyoxyethylene ether.

[0102] The preparation method of propylene glycol polyoxyethylene ether fatty acid ester of the present embodiment comprises the following steps:

[0103] S31, adding 20 parts of propylene glycol polyoxyethylene ether with a polyoxyethylene number of 7 into a reaction kettle, heating to 60° C. under stirring, adding 1 part of p-toluenesulfonic acid and 30 parts of stearic acid, heating to 150° C. and reacting for 4 hours to obtain a crude product of propylene glycol polyoxyethylene ether fatty acid ester;

[0104] S32, adding a sufficient amount of 10wt% sodium hydroxide solution to neutralize the crude product of propylene glycol polyoxyethylene ether fatty acid ester, washing the crude product of propylene glycol polyoxyethylene ether fatty acid ester with a saturated sodium chloride solution, and purifying to obtain propylene glycol polyoxyethylene ether fatty acid ester.

[0105] Example 4, a refining agent for improving penetration emulsification in this example is prepared from the following ingredients in parts by weight: 17 parts of pine alcohol polyoxypropylene polyoxyethylene ether, 17 parts of sodium alkyl sulfonate, 17 parts of rosin amine polyoxyethylene ether, 14 parts of propylene glycol polyoxyethylene ether fatty acid ester and 40 parts of deionized water.

[0106] The polyoxypropylene number of the pine alcohol polyoxypropylene polyoxyethylene ether is 2, the polyoxyethylene number is 18, the alkyl carbon chain number of the sodium alkyl sulfonate is 12, the polyoxyethylene number of the rosin amine polyoxyethylene ether is 18, and the polyoxyethylene number of the propylene glycol polyoxyethylene ether fatty acid ester is 4.

[0107] A method for preparing a refining agent for improving penetration emulsification in this embodiment includes the following steps:

[0108] S1, adding pine alcohol polyoxypropylene polyoxyethylene ether, sodium alkyl sulfonate, rosin amine polyoxyethylene ether and propylene glycol polyoxyethylene ether fatty acid ester into a mixing kettle in sequence, stirring at 40° C. for 50 min to obtain a mixed solution;

[0109] S2. Add deionized water into the mixed solution for dilution to obtain a refining agent for improving penetration and emulsification.

[0110] The preparation method of pinene alcohol polyoxypropylene polyoxyethylene ether of this embodiment comprises the following steps:

[0111] S11, add 20 parts of terpineol into the reactor, introduce nitrogen to replace the air 3 times, heat to 90°C and dehydrate under negative pressure for 1 hour, then add 22 parts of propylene oxide, heat to 130°C and react for 3 hours;

[0112] S12, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted propylene oxide to obtain a terpineol polyoxypropylene ether intermediate product;

[0113] S13, adding 1 part of sodium hydroxide and 105 parts of ethylene oxide to the intermediate product of pinene alcohol polyoxypropylene ether, raising the temperature to 130° C. for reaction for 4 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude product of pinene alcohol polyoxypropylene polyoxyethylene ether;

[0114] S14, neutralizing the crude product of pineol polyoxypropylene polyoxyethylene ether with 10wt% hydrochloric acid to neutrality, and filtering to obtain pineol polyoxypropylene polyoxyethylene ether.

[0115] The preparation method of the rosin amine polyoxyethylene ether of this embodiment comprises the following steps:

[0116] S21, add 20 parts of dehydroabietin amine into the reaction kettle, introduce nitrogen to replace the air 3 times, heat to 80°C and dehydrate under negative pressure for 1 hour, then add 7 parts of the first part of ethylene oxide, heat to 130°C and react for 3 hours;

[0117] S22, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted ethylene oxide to obtain a rosin amine polyoxyethylene ether intermediate product;

[0118] S23, adding 1 part of sodium hydroxide and 50 parts of the second part of ethylene oxide to the rosin amine polyoxyethylene ether intermediate product, heating to 130° C. and aging for 5 hours, and removing unreacted ethylene oxide in vacuo after cooling to obtain a crude rosin amine polyoxyethylene ether;

[0119] S24, neutralizing the crude rosin amine polyoxyethylene ether with 10 wt % hydrochloric acid until neutral, and filtering to obtain the rosin amine polyoxyethylene ether.

[0120] The preparation method of propylene glycol polyoxyethylene ether fatty acid ester of the present embodiment comprises the following steps:

[0121] S31, adding 20 parts of propylene glycol polyoxyethylene ether with a polyoxyethylene number of 4 into a reaction kettle, heating to 60° C. under stirring, adding 2 parts of zinc oxide and 36 parts of myristic acid, and then heating to 150° C. for reaction for 4 hours to obtain a crude product of propylene glycol polyoxyethylene ether fatty acid ester;

[0122] S32, adding a sufficient amount of 10wt% sodium bicarbonate solution to the crude product of propylene glycol polyoxyethylene ether fatty acid ester to neutralize it, washing the crude product of propylene glycol polyoxyethylene ether fatty acid ester with a saturated sodium chloride solution, and purifying to obtain propylene glycol polyoxyethylene ether fatty acid ester.

[0123] Example 5. A refining agent for improving penetration and emulsification in this example is prepared from the following ingredients in parts by weight: 20 parts of pine alcohol polyoxypropylene polyoxyethylene ether, 15 parts of sodium alkyl sulfonate, 20 parts of rosin amine polyoxyethylene ether, 10 parts of propylene glycol polyoxyethylene ether fatty acid ester and 30 parts of deionized water.

[0124] The polyoxypropylene number of the pine alcohol polyoxypropylene polyoxyethylene ether is 3, the polyoxyethylene number is 15, the alkyl carbon chain number of the sodium alkyl sulfonate is 16, the polyoxyethylene number of the rosin amine polyoxyethylene ether is 16, and the polyoxyethylene number of the propylene glycol polyoxyethylene ether fatty acid ester is 4.

[0125] A method for preparing a refining agent for improving penetration emulsification in this embodiment includes the following steps:

[0126] S1, adding pine alcohol polyoxypropylene polyoxyethylene ether, sodium alkyl sulfonate, rosin amine polyoxyethylene ether and propylene glycol polyoxyethylene ether fatty acid ester into a mixing kettle in sequence, stirring at 40° C. for 40 minutes to obtain a mixed solution;

[0127] S2. Add deionized water into the mixed solution for dilution to obtain a refining agent for improving penetration and emulsification.

[0128] The preparation method of pinene alcohol polyoxypropylene polyoxyethylene ether of this embodiment comprises the following steps:

[0129] S11, add 20 parts of terpineol into the reactor, introduce nitrogen to replace the air 3 times, heat to 90°C and dehydrate under negative pressure for 1 hour, then add 25 parts of propylene oxide, heat to 130°C and react for 3 hours;

[0130] S12, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted propylene oxide to obtain a terpineol polyoxypropylene ether intermediate product;

[0131] S13, adding 2 parts of sodium hydroxide and 85 parts of ethylene oxide to the intermediate product of pinene alcohol polyoxypropylene ether, heating to 130° C. for reaction for 4 hours, and removing unreacted ethylene oxide in vacuo after cooling to obtain a crude product of pinene alcohol polyoxypropylene polyoxyethylene ether;

[0132] S14, neutralizing the crude product of pineol polyoxypropylene polyoxyethylene ether with 10wt% hydrochloric acid until neutral, and filtering to obtain pineol polyoxypropylene polyoxyethylene ether.

[0133] The preparation method of the rosin amine polyoxyethylene ether of this embodiment comprises the following steps:

[0134] S21, add 20 parts of dehydroabietin amine into the reaction kettle, introduce nitrogen to replace the air 3 times, heat to 80°C and dehydrate under negative pressure for 1 hour, then add 6 parts of the first part of ethylene oxide, heat to 130°C and react for 3 hours;

[0135] S22, after the reaction is completed, the temperature is lowered to 80° C., and nitrogen is introduced to remove unreacted ethylene oxide to obtain a rosin amine polyoxyethylene ether intermediate product;

[0136] S23, adding 1 part of sodium hydroxide and 45 parts of the second part of ethylene oxide to the rosin amine polyoxyethylene ether intermediate product, heating to 130° C. and aging for 4 hours, and removing unreacted ethylene oxide in vacuo after cooling to obtain a crude rosin amine polyoxyethylene ether;

[0137] S24, neutralizing the crude rosin amine polyoxyethylene ether with 10 wt % hydrochloric acid until neutral, and filtering to obtain the rosin amine polyoxyethylene ether.

[0138] The preparation method of propylene glycol polyoxyethylene ether fatty acid ester of the present embodiment comprises the following steps:

[0139] S31, adding 20 parts of propylene glycol polyoxyethylene ether with a polyoxyethylene number of 4 into a reaction kettle, heating to 60° C. under stirring, adding 1 part of p-toluenesulfonic acid and 50 parts of stearic acid, heating to 130° C. and reacting for 4 hours to obtain a crude product of propylene glycol polyoxyethylene ether fatty acid ester;

[0140] S32, adding a sufficient amount of 10wt% sodium bicarbonate solution to the crude product of propylene glycol polyoxyethylene ether fatty acid ester to neutralize it, washing the crude product of propylene glycol polyoxyethylene ether fatty acid ester with a saturated sodium carbonate solution, and purifying to obtain propylene glycol polyoxyethylene ether fatty acid ester.

[0141] Comparative Example 1: This comparative example differs from Example 1 in that pineol polyoxypropylene polyoxyethylene ether is replaced with dodecyl polyoxypropylene polyoxyethylene ether.

[0142] Comparative Example 2: This comparative example differs from Example 1 in that the number of polyoxyethylenes in the rosin amine polyoxyethylene ether is changed to 10.

[0143] Comparative Example 3: This comparative example differs from Example 1 in that propylene glycol polyoxyethylene ether fatty acid ester is not added.

[0144] Performance Testing

[0145] Preparation of treatment liquid: 2 g / L of sodium hydroxide, 7 g / L of hydrogen peroxide and 1.0 g / L of the scouring agent prepared in each example and comparative example were mixed to prepare the treatment liquid.

[0146] Fabric pretreatment: The cotton fabric was pretreated by immersion method, with the treatment temperature set at 80°C, the treatment time 60 min, and the bath ratio 1:25. After the fabric pretreatment, the fabric was washed with hot water at 80-90°C and neutralized with acid, and dried to obtain the test fabric.

[0147] Whiteness test: Determine the whiteness of the test fabric according to GB / T8424.2-2001 "Instrumental evaluation method for relative whiteness of textile color fastness tests".

[0148] Capillary effect test: According to FZ / T 01071-2008 "Test method for capillary effect of textiles", the capillary effect of the test fabric is measured.

[0149] Breaking strength test: The breaking strength of the test fabric is measured according to GB / T 3923.1-2013 "Tensile properties of textile fabrics Part 1: Determination of breaking strength and elongation at break by strip method".

[0150] Wetting performance test: The wetting performance test of the scouring agent was carried out according to the method specified in GB / T 11983-2008 "Determination of the wetting power of surfactants - sinking method", and the fabric used for wetting was a cotton canvas piece.

[0151] Emulsification performance test: The emulsification performance test of the scouring agent was carried out according to the method specified in GB / T 11543-2008 "Test method for properties of medium and high viscosity emulsions of surfactants and evaluation method for their emulsification ability", and the test reagent was liquid paraffin.

[0152] The test results are shown in Table 1:

[0153] Table 1

[0154]

[0155] From the data in Table 1, it can be seen that the whiteness of the test fabric treated with the treatment solution prepared in Examples 1 to 5 is between 73.5% and 75.8%, and the capillary effect is between 12.4 and 13.3 cm×30 min. -1 The breaking strength is between 314 and 319 N, indicating that the scouring agent prepared by the present invention can effectively remove impurities in the fabric after being applied to the fabric pretreatment process, and the treated fabric has good whiteness, excellent hair effect, and small fabric strength loss; the canvas wetting time of the scouring agent prepared in Examples 1 to 5 is between 22 and 26 s, indicating that the scouring agent prepared by the present invention has excellent penetrating wetting performance, and the emulsification time of the scouring agent prepared in Examples 1 to 5 in liquid paraffin is 134 to 140 s, indicating that the scouring agent prepared by the present invention has excellent emulsifying performance, further indicating that the scouring agent prepared by the present invention has excellent penetrating emulsifying performance.

[0156] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

[0157] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A refining agent for improving penetration emulsification, characterized in that: The invention is prepared from the following ingredients in parts by weight: 15-20 parts of pine alcohol polyoxypropylene polyoxyethylene ether, 15-25 parts of sodium alkyl sulfonate, 10-15 parts of rosin amine polyoxyethylene ether, 10-20 parts of propylene glycol polyoxyethylene ether fatty acid ester and 20-50 parts of deionized water; The polyoxypropylene number of the pine alcohol polyoxypropylene polyoxyethylene ether is between 1 and 3, the polyoxyethylene number is between 15 and 20, the alkyl carbon chain number of the sodium alkyl sulfonate is between 12 and 18, the polyoxyethylene number of the rosin amine polyoxyethylene ether is between 15 and 20, and the polyoxyethylene number of the propylene glycol polyoxyethylene ether fatty acid ester is between 4 and 7.

2. The method for preparing a refining agent for improving penetration emulsification according to claim 1, characterized in that: The steps include: S1, add pine alcohol polyoxypropylene polyoxyethylene ether, sodium alkyl sulfonate, rosin amine polyoxyethylene ether and propylene glycol polyoxyethylene ether fatty acid ester into a mixing kettle in sequence, and stir at 40-50° C. for 30-50 minutes to obtain a mixed solution; S2, adding deionized water to the mixed solution to dilute it to obtain a refining agent that improves penetration and emulsification; The preparation method of pineol polyoxypropylene polyoxyethylene ether comprises the following steps: S11, add terpineol into the reactor, introduce nitrogen to replace the air 3 times, heat to 80-90°C and dehydrate under negative pressure for 0.5-1h, add propylene oxide, heat to 120-140°C and react for 3-4h; S12, after the reaction is completed, the temperature is lowered to 70-80°C, and nitrogen is introduced to remove unreacted propylene oxide to obtain a terpineol polyoxypropylene ether intermediate product; S13, adding the first catalyst and ethylene oxide to the pinene alcohol polyoxypropylene ether intermediate product, raising the temperature to 120-140° C. for reaction for 3-5 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude product of pinene alcohol polyoxypropylene polyoxyethylene ether; S14, neutralizing the crude product of pineol polyoxypropylene polyoxyethylene ether with 10wt% hydrochloric acid until neutral, and filtering to obtain pineol polyoxypropylene polyoxyethylene ether; The preparation method of rosin amine polyoxyethylene ether comprises the following steps: S21, adding rosin amine compounds into the reaction kettle, introducing nitrogen to replace air 3 times, heating to 80-90°C for negative pressure dehydration for 0.5-1h, adding the first part of ethylene oxide, heating to 120-140°C for reaction for 3-4h; S22, after the reaction is completed, the temperature is lowered to 70-80°C, and nitrogen is introduced to remove unreacted ethylene oxide to obtain a rosin amine polyoxyethylene ether intermediate product; S23, adding the second catalyst and the second part of ethylene oxide to the rosin amine polyoxyethylene ether intermediate product, raising the temperature to 120-140° C. and aging for 3-5 hours, and removing the unreacted ethylene oxide in vacuo after cooling to obtain a crude rosin amine polyoxyethylene ether; S24, neutralizing the crude rosin amine polyoxyethylene ether with 10 wt % hydrochloric acid until neutral, and filtering to obtain the rosin amine polyoxyethylene ether.

3. The method for preparing a refining agent for improving penetration emulsification according to claim 2, characterized in that: The first catalyst in S13 is one or more combinations of sodium hydroxide, potassium hydroxide and sodium hydride. The weight parts of each substance used in the preparation process of pineol polyoxypropylene polyoxyethylene ether are 20 parts of pineol, 8-25 parts of propylene oxide, 0.5-2 parts of the first catalyst and 85-115 parts of ethylene oxide.

4. The method for preparing a refining agent for improving penetration emulsification according to claim 2, characterized in that: The rosin amine compound in S21 is one or both of rosin amine and dehydrorosin amine, the second catalyst in S23 is one or more combinations of sodium hydroxide, potassium hydroxide and sodium hydride, and the weight parts of each substance used in the preparation process of the rosin amine polyoxyethylene ether are 20 parts of rosin amine, 6-7 parts of the first part of ethylene oxide, 0.5-2 parts of the second catalyst and 40-60 parts of the second part of ethylene oxide.

5. The method for preparing a refining agent for improving penetration emulsification according to claim 2, characterized in that: The preparation method of propylene glycol polyoxyethylene ether fatty acid ester comprises the following steps: S31, adding propylene glycol polyoxyethylene ether into a reaction kettle, heating to 50-60° C. under stirring, adding an esterification catalyst and fatty acid, heating to 130-150° C. and reacting for 3-4 hours to obtain a crude product of propylene glycol polyoxyethylene ether fatty acid ester; S32, adding a sufficient amount of alkaline solution to the crude product of propylene glycol polyoxyethylene ether fatty acid ester to neutralize it, washing the crude product of propylene glycol polyoxyethylene ether fatty acid ester with a saturated salt solution, and purifying it to obtain propylene glycol polyoxyethylene ether fatty acid ester.

6. The method for preparing a refining agent for improving penetration emulsification according to claim 5, characterized in that: The esterification catalyst in S31 is one or more combinations of p-toluenesulfonic acid, potassium hydroxide and zinc oxide, the fatty acid is one or more combinations of lauric acid, myristic acid, palmitic acid and stearic acid, the alkaline solution in S32 is one or more combinations of sodium bicarbonate solution, potassium bicarbonate solution, sodium hydroxide solution and potassium hydroxide solution, the saturated salt solution is one or more combinations of saturated sodium chloride solution, saturated calcium chloride solution and saturated sodium carbonate solution, and the weight parts of each substance used in the preparation process of the propylene glycol polyoxyethylene ether fatty acid ester are 20 parts of propylene glycol polyoxyethylene ether, 0.5-2 parts of esterification catalyst and 20-50 parts of fatty acid.

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