A system for preparing rosin polyoxyethylene ether and a method for preparing rosin polyoxyethylene ether using the same
Through the improved rosin polyoxyethylene ether preparation system, the use of crushing and screening devices combined with reactors has solved the problems of long production cycle and high solvent loss in the existing technology, and achieved efficient preparation of rosin polyoxyethylene ether, with a narrow molecular weight distribution and excellent emulsification properties.
Patent Information
- Application Number
- CN202411343100.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-25
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2044-09-25
AI Technical Summary
The existing synthesis methods of rosin polyoxyethylene ether have the problems of long production cycle, high solvent loss, high cost and wide product molecular weight distribution.
A preparation system including first and second crushing devices, a screening device, a conveying device and a reactor is used. The rosin is first crushed and screened, and then dehydrated and reacted with ethylene oxide in two reactors respectively. This shortens the melting time and improves the heating uniformity to prepare solvent-free rosin polyoxyethylene ether.
The rosin melting time is greatly shortened, the product molecular weight distribution is narrow, the emulsification performance is excellent, the production cost is reduced, and the product quality is improved.
Smart Images

Figure CN119281228B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of polyether synthesis, and particularly relates to a preparation system of rosin polyoxyethylene ether and a method for preparing rosin polyoxyethylene ether by using the same. Background Art
[0002] Rosin polyoxyethylene ether is a nonionic surfactant synthesized by reacting rosin with ethylene oxide (EO) in the presence of a catalyst. Rosin's primary component is abietic acid, which contains tricyclic diterpenes. Ethoxylated rosin polyoxyethylene ethers exhibit strong emulsifying and dispersing abilities, significantly reducing the surface tension of aqueous solutions. They can be used directly or in combination to create various industrial and household detergents. They can also be used directly as an emulsifier for various oils and skincare products, and as an emulsifier for emulsion-type contact insecticides. As a detergent, rosin polyoxyethylene ethers possess superior detergency compared to fatty alcohol polyoxyethylene ethers. Their aqueous solutions lack the greasy, alkaline feel of laundry detergents and soaps, produce minimal foam, rinse clean, and are easy to rinse. They are also mild and non-drying to the skin and hands, making them excellent detergent materials. Rosin is a natural product and a readily available, inexpensive, renewable, and bioavailable raw material.
[0003] The synthesis method of rosin polyoxyethylene ether has been reported. In 1996, Wang Yan and Zhou Yonghong published "Synthesis and Properties of Rosin Acid Polyoxyethylene Ester" in the journal of "Chemistry and Industry of Forest Products", which studied the reaction of rosin acid and ethylene oxide after dehydration at 180°C. After the reaction was completed, the temperature was lowered to below 100°C for bleaching and neutralization to obtain rosin acid polyoxyethylene ester with different polymerization degrees and compare their properties. In 2002, Zheng Naixin et al. published "Synthesis of Rosin Acid Polyoxyethylene Ester (PORE) and Its Application in Paper Sizing Agent" in "Dezhou University Journal", which studied the synthesis of rosin acid polyoxyethylene ester by adding ethylene oxide after dehydration at 140-180°C with KOH as catalyst. In 2004, Zhou Cun et al. published "Synthesis Process and Performance of Rosin Acid Polyoxyethylene Ester" in "Tianjin University of Technology Journal", which used 0.3%-0.5% KOH as catalyst, dehydrated at 105-120°C under vacuum, then added ethylene oxide at 140-180°C, and after the reaction was completed, added acid for neutralization, then added adsorbent for filtration to obtain rosin polyoxyethylene ester product. In 2012, Che Wencheng et al. published "Synthesis of Rosin Polyoxyethylene Ether Nonionic Surfactant" in "Chemical Technology and Development", which used KOH and self-made catalyst B to react at 120°C, 150°C, 180°C, and 200°C to obtain products with different polymerization degrees and compared them. Patent CN201210037761.5 discloses a method for preparing rosin polyoxyethylene ether nonionic surfactant: using 20%-110% ethanol or acetone by weight of solid rosin as solvent, 1-5‰ potassium hydroxide or sodium hydroxide by weight of solid rosin as catalyst, vacuuming ethanol or acetone at 90-120°C, then adding ethylene oxide at 125-185°C, and after the reaction is completed, adding glacial acetic acid to neutralize the pH value to 6.5-7.5 to obtain rosin polyoxyethylene ether product.
[0004] The synthesis methods provided by the prior art in this field mainly include two types: 1. Using alkali metal hydroxides such as KOH and NaOH as catalysts, rosin acid and ethylene oxide react at 120-180°C to produce rosin polyoxyethylene ether; 2. Using a solvent to dissolve rosin acid, adding the catalyst, vacuum-evacuating ethanol or acetone at 90-120°C, adding ethylene oxide to react at 125-185°C, and adding glacial acetic acid to neutralize the pH to 6.5-7.5 after the reaction is complete to produce the finished rosin polyoxyethylene ether. Both synthesis methods have their shortcomings. Rosin acid itself is solid with a high melting point, and rosin acid available on the market is in the form of amorphous large blocks or large particles of uneven size. Method 1 uses it to synthesize rosin polyoxyethylene ether, which takes a lot of time (production takes more than 7 hours) to melt the block rosin into liquid, then dehydrate and add ethylene oxide to the polymerization process, resulting in a long production cycle and a wide molecular weight distribution of the product. Method 2 uses a solvent to dissolve the rosin acid, then heats the process to remove the solvent before dehydrating the product and adding the ethylene oxide polymerization step. This method results in the loss of volatile solvent, resulting in high production costs and environmental pollution. Solvent residue also affects the emulsification properties of the product.
[0005] Therefore, there is an urgent need to provide a preparation method of rosin polyoxyethylene ether, which can prepare rosin polyoxyethylene ether with narrow molecular weight distribution and excellent emulsification performance; and can shorten the time of synthesizing chemical materials and reduce production costs. Summary of the Invention
[0006] The present invention aims to address at least one of the technical problems existing in the aforementioned prior art. To this end, the present invention provides a system for preparing rosin polyoxyethylene ether and a method for preparing rosin polyoxyethylene ether using the system. The system provided by the present invention can produce solvent-free rosin polyoxyethylene ether with a narrow molecular weight distribution, shorten the synthesis time, and reduce production costs.
[0007] The present invention provides a preparation system of rosin polyoxyethylene ether, comprising:
[0008] An oligomer preparation system includes a first crushing device, a first screen device, a first conveying device, and a first reactor; a discharge port A of the first crushing device is located above the first screen device, and material enters the first screen device through the discharge port A; a receiving port of the first conveying device is located below the first screen device and is connected to the feed port of the first reactor, for collecting screened material and conveying it to the first reactor;
[0009] A polyether preparation system comprising a second crushing device, a second screen device, a second conveying device, and a second reactor; a discharge port B of the second crushing device is located above the second screen device, and material enters the second screen device through the discharge port B; a receiving port of the second conveying device is located below the second screen device and is connected to a feed port of the second reactor, for collecting screened material and conveying it to the second reactor;
[0010] A third conveying device is connected to the first reactor and the second reactor, and is used for conveying oligomers.
[0011] Preferably, the first reactor is provided with a gas introduction device and an exhaust device.
[0012] Preferably, the second reactor is provided with a gas introduction device and an exhaust device.
[0013] Preferably, the first and second reaction vessels are further provided with a vacuum pump, such as a vacuum pump. It is understood that the first and second reaction vessels may be provided with a vacuum pump respectively or may share a vacuum pump.
[0014] Preferably, a stirring device is further provided in the first reactor.
[0015] Preferably, a stirring device is further provided in the second reactor.
[0016] The invention also provides a preparation method of rosin polyoxyethylene ether.
[0017] Specifically, a method for preparing rosin polyoxyethylene ether, using the above-mentioned preparation system, comprises the following steps:
[0018] (1) crushing and sieving a portion of rosin, mixing it with catalyst A, and dehydrating it; then heating it and continuously introducing ethylene oxide to react to obtain rosin polyoxyethylene ether oligomers;
[0019] (2) crushing and sieving another portion of rosin, adding it to the rosin polyoxyethylene ether oligomer prepared in step (1), adding catalyst B, and dehydrating; then heating, continuously introducing ethylene oxide to react, and preparing rosin polyoxyethylene ether.
[0020] Preferably, the rosin comprises one of hydrogenated rosin, abietic acid or disproportionated rosin.
[0021] Preferably, in step (1), the weight ratio of the portion of rosin to the ethylene oxide is 1:0.25-0.72.
[0022] Preferably, the catalyst A in step (1) and the catalyst B in step (2) are each independently selected from at least one of potassium hydroxide, sodium hydroxide, potassium methoxide, and sodium methoxide. The amount of the catalyst A used in step (1) is 0.03% to 0.2% of the total weight of the rosin and the ethylene oxide. The amount of the catalyst B used in step (2) is 0.03% to 0.2% of the total weight of the rosin and the ethylene oxide.
[0023] Preferably, the dehydration process in step (1) is: dehydration for 0.5-2h at 100-130°C and vacuum ≥-0.098MPa.
[0024] Preferably, the reaction temperature in step (1) is 120-170° C., the reaction pressure is -0.05-0.35 MPa, and the reaction time is 2-6 h.
[0025] Preferably, in step (2), the weight ratio of the rosin polyoxyethylene ether oligomer to the other portion of rosin and the ethylene oxide is 1:(0.5-1.5):(1.0-10.0).
[0026] Preferably, the dehydration process in step (2) is: dehydration for 0.5-2h at 100-130°C and vacuum ≥-0.098MPa.
[0027] Preferably, the reaction temperature in step (2) is 120-170° C., the reaction pressure is -0.05-0.35 MPa, and the reaction time is 2-10 h.
[0028] Preferably, the sieving process in step (1) and step (2) is: sieving through a sieve with a mesh diameter of 0.2-0.5 cm.
[0029] More specifically, a method for preparing rosin polyoxyethylene ether is prepared using the above-mentioned preparation system. The preparation method is divided into two steps:
[0030] (1) A portion of rosin in block or granular form is crushed and sieved, and then added to the first reactor. After the feeding is completed and the catalyst is added, the feeding gate valve is closed, and the vacuum is evacuated to a vacuum of ≥-0.098 MPa in the first reactor, and then the vacuum is closed. N2 is filled to a pressure of 0.02 MPa in the first reactor, and then the vacuum is evacuated to ≥-0.098 MPa. Stirring is started and the temperature is raised. After the temperature reaches the specified temperature, the vacuum is evacuated to ≥-0.098 MPa for dehydration for 1 hour. After dehydration, the vacuum valve is closed, and a certain amount of ethylene oxide is continuously introduced into the reactor for reaction after the temperature is raised. After the reaction is completed, the temperature is lowered to obtain rosin polyoxyethylene ether oligomers.
[0031] (2) Add the rosin polyoxyethylene ether oligomer prepared in step (1) to the second reactor, crush and sieve the other part of the block or granular rosin, and add it to the second reactor. After the rosin is added, the feed gate valve is closed after the catalyst is added, and the vacuum in the first reactor is evacuated to -0.098 MPa, and then the vacuum is closed. N2 is filled to the pressure in the reactor to 0.02 MPa, and then the vacuum is evacuated to ≥-0.098 MPa. Stirring is started and the temperature is raised at the same time. After the temperature is raised to the specified temperature, the vacuum is ≥-0.098 MPa and dehydrated for 1 hour. After dehydration is completed, the vacuum valve is closed, and a certain amount of ethylene oxide is continuously introduced into the reactor for reaction after the temperature is raised. After the reaction is completed, the temperature is lowered to obtain the rosin polyoxyethylene ether finished product.
[0032] Compared with the prior art, the present invention has the following beneficial effects:
[0033] 1. The preparation system of the present invention can significantly shorten the rosin melting time to less than one-third of that of conventional methods. The preparation system can also increase the heating area of the rosin, allowing for uniform heating. The resulting product has a narrow molecular weight distribution, light color, good emulsification properties, and excellent quality.
[0034] 2. The preparation method of allyl alcohol polyoxyethylene ether provided by the present invention adopts the above-mentioned preparation system for preparation. First, rosin polyoxyethylene ether oligomers are prepared. Then, the rosin polyoxyethylene ether oligomers and the rosin mixture are used as starting materials to prepare allyl alcohol polyoxyethylene ether. The rosin melting time is greatly shortened, the materials are heated evenly, and the obtained product has a narrow molecular weight distribution, light color, good emulsification performance, is solvent-free, and has excellent quality. In addition, this preparation method can effectively reduce production costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0035] Figure 1 Schematic diagram of the structure of the preparation system of rosin polyoxyethylene ether in an embodiment of the present invention;
[0036] Description of Figure Numbers:
[0037] Oligomer preparation system 100, first crushing device 110, first screen device 120, first conveying device 130, first reactor 140, first stirring device 141;
[0038] Polyether preparation system 200, second crushing device 210, second screening device 220, second conveying device 230, second reactor 240, second stirring device 241;
[0039] A third conveying device 300;
[0040] Vacuuming device 400. DETAILED DESCRIPTION
[0041] In order to make the technical solution of the present invention more clearly understood by those skilled in the art, the following examples are given for illustration. It should be noted that the following examples do not limit the scope of protection claimed by the present invention.
[0042] Unless otherwise specified, the raw materials and reagents used in the following examples and comparative examples can be obtained from conventional commercial sources or by existing known methods.
[0043] An embodiment of the present invention provides a system for producing rosin polyoxyethylene ether, comprising: an oligomer production system 100, a polyether production system 200, and a third conveying device 300. The third conveying device 300 is connected to a first reactor 140 and a second reactor 240 for conveying oligomers. The oligomer production system 100 includes a first crushing device 110, a first screen device 120, a first conveying device 130, and the first reactor 140. The discharge port A of the first crushing device 110 is located above the first screen device 120, through which material enters the first screen device 120. The receiving port of the first conveying device 130 is located below the first screen device 120 and connected to the feed port of the first reactor 140, collecting the screened material and conveying it to the first reactor 140. The first reactor 140 is equipped with a gas inlet and exhaust device. A stirring device 141 is also provided within the first reactor 140 for stirring the material.
[0044] The polyether preparation system 200 includes a second crushing device 210, a second screening device 220, a second conveying device 230 and a second reactor 240; the discharge port B of the second crushing device 210 is located above the second screening device 220, and the material enters the second screening device 220 through the discharge port B; the receiving port of the second conveying device 230 is located below the second screening device 220 and is connected to the feed port of the second reactor 140, for collecting the screened material and conveying it to the second reactor 240; the second reactor 240 is provided with a gas inlet device and an exhaust device, and the second reactor 240 is also provided with a stirring device 241 for stirring the material.
[0045] More specifically, a vacuum pump 400, such as a vacuum pump, is further provided on the first reactor 140 and the second reactor 240. It is understood that the first reactor 140 and the second reactor 240 can be provided with a vacuum pump 400 respectively, or can share the vacuum pump 400.
[0046] The production system of the embodiment of the present invention includes an oligomer production system 100 and a polyether production system 200. The oligomer production system 100 first produces rosin polyoxyethylene ether oligomers, which are then transported to the polyether production system 200 via a third conveying device 300 to produce the rosin polyoxyethylene ether. During the oligomer production process, large rosin blocks are first crushed using a first crushing device 110. Small particles with a particle size of less than 0.5 cm are screened using a first screening device 120 and fed into a first reactor 140. The large particles are then transported through the first screening device 120 into the first crushing device 110 for further crushing, thereby reducing the large rosin blocks to small particles for use in synthesizing rosin polyoxyethylene ether oligomers. During the polyether preparation process, rosin polyoxyethylene ether oligomer is transported to the second reactor 240 via the third transport device 300. The rosin in bulk or granular form is crushed by the second crushing device 210. The rosin is then screened by the second sieve device 220 to remove small particles with a diameter of less than 0.5 cm. These particles are then fed into the second reactor 240. Large particles are then carried through the second sieve device 220 to the second crushing device 210 for further crushing. This reduces the bulk rosin to small particles for the synthesis reaction.
[0047] During the preparation of oligomers and polyethers, the pressure and vacuum level of the first reactor 140 and the second reactor 240 are controlled by a gas introduction device, an exhaust device, and a vacuum device 400. Specifically, nitrogen can be introduced into the reactors by the gas introduction device, exhausted by the exhaust device, and the vacuum level in the reactors can be controlled by the vacuum device 400.
[0048] The preparation system of the embodiment of the present invention can increase the heating area of rosin by crushing and sieving the rosin first, and reduce the resistance when stirring the reactor, making it easier to stir, and the rosin is heated evenly, which greatly shortens the melting time. 3 The reactor is equipped with a 3-ton rosin reactor. For example, 0.5 MPa steam is used for heating. The large pieces of rosin that are not normally processed need 10-12 hours to melt due to the inability to stir. However, the rosin that has been crushed by the preparation system only needs 3-4 hours to melt. The rosin polyoxyethylene ether oligomer and the crushed rosin are put into the second reactor at a ratio of 1:0.5-1.5 as the starting materials. Since the rosin polyoxyethylene ether oligomer is liquid, mixing with the rosin can increase the lubrication and fluidity of the rosin surface and is more conducive to uniform stirring. When the rosin is heated and melted, the heat exchange area is increased, the heating is uniform, the melting speed is accelerated, and the dark color of the product caused by severe local heating is avoided. 3 For example, if 2 tons of rosin and 1.3 tons of rosin polyoxyethylene ether oligomer mixture is added to the kettle, it only takes 1.5-2 hours to melt, while the normal 12m 3 The kettle was filled with 2 tons of uncrushed rosin. Since it could not be stirred, it took 7-9 hours to melt, which greatly shortened the melting time.
[0049] Under high temperature conditions, the C=C double bonds and C-C single bonds in rosin are oxidized and cleaved to form aldehydes and ketones, which are then converted into byproducts of varying molecular weights. At high temperatures, some of these aldehydes and ketones react with each other to form acetals or ketals, producing substances of varying molecular weights. These aldehydes, ketones, and acetals / ketals in the raw material react together with ethylene oxide, resulting in a product with a wide molecular weight distribution and a dark color. The preparation system of the present invention significantly shortens the rosin melting time and reduces the probability of rosin oxidation producing aldehydes, ketones, and acetals / ketals as byproducts. The resulting rosin polyoxyethylene ether product, synthesized by reacting with ethylene oxide, has a narrow molecular weight distribution and a light color, significantly improving product quality.
[0050] The embodiment of the present invention also provides a method for preparing rosin polyoxyethylene ether, which is prepared using the above preparation system.
[0051] Preparation of the reactors before preparation: First, clean, purge, and dry the preparation system until it is clean and dry; then dry each reactor, cool it to room temperature, and set aside. The following examples illustrate the present invention but are not intended to limit its scope. The molecular weights referred to in the Examples and Comparative Examples are Mn (number average molecular weight, measured by gel permeation chromatography (GPC)) and the molecular weight distribution coefficient D (measured by gel permeation chromatography (GPC)).
[0052] Example 1
[0053] Preparation of rosin polyoxyethylene ether oligomers, the steps are as follows:
[0054] 3000kg of hydrogenated rosin is put into 12m3 of pulverized rosin after passing through the patented preparation system of this invention. 3 In the first reactor, add 4kg of KOH catalyst and close the feeding gate valve. Evacuate the reactor until the vacuum reaches -0.098Mpa, then close the vacuum, fill with N2 until the pressure in the reactor reaches 0.02MPa, and then evacuate to ≥-0.098MPa. Then start stirring and heat the material (control the heating steam at 0.5MPa). After the temperature rises to 115°C, dehydrate under vacuum ≥-0.098MPa for 1h. After dehydration is completed, close the vacuum valve, raise the temperature to 130°C, and continue to introduce a certain amount of ethylene oxide to react. The reaction temperature is controlled at 150°C and the reaction pressure is controlled at ≤0.35. After the reaction is completed, cool to 60°C to obtain rosin polyoxyethylene ether oligomer.
[0055] Examples 2-4
[0056] The process conditions of Example 1 remain unchanged, and the amount of raw materials, ethylene oxide, and the type and amount of catalyst are adjusted. The raw materials used and the test results are shown in Table 1.
[0057] Table 1
[0058]
[0059] Example 5
[0060] Preparation of rosin polyoxyethylene ether, the steps are as follows:
[0061] 2000kg of hydrogenated rosin and 1300kg of rosin polyoxyethylene ether oligomer obtained in Example 1 were put into the second reactor through the preparation system of the present invention. 3 In the second reactor, 7.6 kg of KOH catalyst was added, and the feeding gate valve was closed. Then, 1300 kg of rosin polyoxyethylene ether oligomer obtained in Example 1 was pressed into the second reactor from the bottom pipe of the first reactor. After the vacuum in the reactor was evacuated to -0.098 MPa, the vacuum was turned off, and N2 was filled to the pressure in the reactor to 0.02 MPa. After evacuating to ≥ -0.098 MPa, stirring was started, and the material was heated (heating steam was controlled at 0.5 MPa). After the temperature was raised to 115 ° C, the vacuum was ≥ -0.098 MPa for dehydration for 1 hour. After dehydration was completed, the vacuum valve was closed, and the temperature was raised to 130 ° C. After that, 5658 kg of ethylene oxide was continuously introduced into the reactor for reaction. The reaction temperature was controlled at 150 ° C. The reaction was controlled at a pressure of ≤ 0.35. After the reaction was completed, the temperature was cooled to 60 ° C and the material was discharged to obtain the rosin polyoxyethylene ether product.
[0062] Examples 6-8
[0063] The process conditions of Example 5 remained unchanged, and the amounts of raw materials, catalyst, and ethylene oxide were adjusted. The raw materials used and the test results are shown in Table 2.
[0064] Table 2
[0065]
[0066]
[0067] Comparative Examples 1-4: Synthesis was performed according to the previously reported method.
[0068] Comparative Example 1
[0069] A method for preparing rosin polyoxyethylene ether comprises the following steps:
[0070] Put 3000kg of un-crushed hydrogenated rosin into the stirring chamber for 12m 3The reactor was added with 9.5 kg of KOH catalyst, and the feeding gate valve was closed. The vacuum was evacuated until the vacuum in the reactor reached -0.098 MPa, and then the vacuum was closed. N2 was filled until the pressure in the reactor reached 0.02 MPa, and then the vacuum was evacuated to ≥-0.098 MPa. At the same time, the temperature of the reactor was increased (the heating steam was controlled at 0.5 MPa). When the stirring could be started, the temperature was increased to 115 ° C, and the vacuum was ≥-0.098 MPa for dehydration for 1 hour. After the dehydration was completed, the vacuum valve was closed, and the temperature was increased to 130 ° C. After that, 6492 kg of ethylene oxide was continuously introduced for reaction. The normal reaction temperature was controlled at 150 ° C, and the reaction was controlled at a pressure of ≤0.35. After the reaction was completed, the temperature was lowered to 60 ° C and the material was discharged to obtain the finished rosin polyoxyethylene ether.
[0071] Comparative Examples 2-4
[0072] The process conditions of Comparative Example 1 remain unchanged, and the amounts of raw materials, ethylene oxide, and the type and amount of catalyst are adjusted. The raw materials used and the test results are shown in Table 3.
[0073] Table 3
[0074]
[0075] As can be seen from Table 1 and Table 3, Examples 1-4 and Comparative Examples 1-2 both used 3000 kg of rosin and were also melted by heating with 0.5 MPa steam. The melting time of the Examples was 3.5-3.8 h, while the melting time of Comparative Example 1-2 was 11.2 h. The melting time of Example 1-4 was only 1 / 3 of that of the Comparative Example.
[0076] As shown in Tables 2 and 3, Examples 5-6 and Comparative Example 3 both used 2000 kg of rosin, and the melting time for Examples 5-6 was only 1.8 hours, less than a quarter of the 8.4 hours required for Comparative Example 3. This demonstrates that the preparation system and method of this patent can significantly shorten the rosin melting time and product production cycle.
[0077] Emulsification performance test: The samples prepared in the examples and comparative examples were prepared into 1% aqueous solutions. 25 mL of each 1% aqueous solution was placed in a 100 mL stoppered graduated cylinder and oscillated with 20 mL of 5# white oil. The mixture was then shaken up and down 30 times and allowed to stand. The time required to separate 10 mL of water was recorded. The results are shown in Table 4.
[0078] Table 4
[0079]
[0080]
[0081] As shown in Tables 2, 3, and 4, the products produced using the preparation method of this patent, Examples 5-8, compared with Comparative Examples 1-4 using a one-step base-catalyzed method using unpulverized rosin, exhibit a narrow molecular weight distribution, a light color, and excellent emulsification properties, with more stable emulsification, provided the catalyst alkalinity, reaction temperature, and theoretical molecular weight of the feed are consistent. Under high temperature conditions, the C=C double bonds and C-C single bonds in the rosin structure undergo oxidation and chain scission to form aldehydes and ketones, which are converted into byproducts of varying molecular weights. At high temperatures, some of these aldehydes and ketones react with each other to form acetals or ketals, producing substances of varying molecular weights. These aldehydes, ketones, and acetals and ketals react with ethylene oxide, resulting in a broad molecular weight distribution and a darker color. Significantly shortening the rosin melting time can significantly reduce the probability of rosin oxidation producing aldehydes, ketones, and acetals and ketals as byproducts. Consequently, the rosin polyoxyethylene ether synthesized by reacting with ethylene oxide has a narrow molecular weight distribution and a light color, significantly improving product quality.
[0082] The above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be determined by the appended claims.
Claims
1. A system for preparing rosin polyoxyethylene ether, characterized in that: include: An oligomer preparation system (100) is provided, comprising a first crushing device (110), a first screen device (120), a first conveying device (130) and a first reactor (140); a discharge port A of the first crushing device (110) is located above the first screen device (120), and materials enter the first screen device (120) through the discharge port A; a receiving port of the first conveying device (130) is located below the first screen device (120) and is connected to a feed port of the first reactor (140), for collecting screened materials and conveying them to the first reactor (140); A polyether preparation system (200) is provided, comprising a second crushing device (210), a second screen device (220), a second conveying device (230), and a second reactor (240); a discharge port B of the second crushing device (210) is located above the second screen device (220), and materials enter the second screen device (220) through the discharge port B; a receiving port of the second conveying device (230) is located below the second screen device (220) and is connected to a feed port of the second reactor (240), for collecting screened materials and conveying them to the second reactor (240); A third conveying device (300) is connected to the first reaction kettle (140) and the second reaction kettle (240) and is used to convey the oligomer.
2. The preparation system according to claim 1, characterized in that: The first reaction kettle (140) and the second reaction kettle (240) are both provided with a gas introduction device and an exhaust device.
3. The preparation system according to claim 1, characterized in that: The first reaction kettle (140) and the second reaction kettle (240) are also provided with a vacuum pumping device (400).
4. A method for preparing rosin polyoxyethylene ether, characterized in that: The preparation method is carried out using the preparation system according to any one of claims 1 to 3, comprising the following steps: (1) crushing and sieving a portion of rosin, mixing it with catalyst A, and dehydrating it; then heating it and continuously introducing ethylene oxide to react to obtain rosin polyoxyethylene ether oligomers; (2) crushing and sieving another portion of rosin, adding it to the rosin polyoxyethylene ether oligomer prepared in step (1), adding catalyst B, and dehydrating; then heating, continuously introducing ethylene oxide to react, and preparing rosin polyoxyethylene ether.
5. The preparation method according to claim 4, characterized in that The rosin includes one of hydrogenated rosin, abietic acid or disproportionated rosin.
6. The preparation method according to claim 4, characterized in that In step (1), the weight ratio of the portion of rosin to the ethylene oxide is 1:(0.25-0.72).
7. The preparation method according to claim 5 or 6, characterized in that: The catalyst A in step (1) and the catalyst B in step (2) are independently selected from at least one of potassium hydroxide, sodium hydroxide, potassium methoxide and sodium methoxide.
8. The preparation method according to claim 7, characterized in that The amount of the catalyst A used is 0.03%-0.2% of the total weight of the rosin and the ethylene oxide in step (1); the amount of the catalyst B used is 0.03%-0.2% of the total weight of the rosin and the ethylene oxide in step (2).
9. The preparation method according to claim 4, characterized in that In step (2), the weight ratio of the rosin polyoxyethylene ether oligomer to the other part of rosin and the ethylene oxide is 1: (0.5-1.5): (1.0-10.0).
10. The preparation method according to claim 4, characterized in that The sieving process in step (1) and step (2) is as follows: sieving through a sieve with a mesh diameter of 0.2-0.5 cm.
Citation Information
Patent Citations
Rosin polyoxyethylene ether nonionic surfactant
CN102614806A
Environment-friendly pulping production process system
CN115305736A
Emulsifying viscosity-reducing drag-reducing agent for produced liquid and preparation method of emulsifying viscosity-reducing drag-reducing agent
CN115595132A