CN111018713A - Pentaerythritol epoxy modified castor oil terminated polymer and preparation method and application thereof - Google Patents
Pentaerythritol epoxy modified castor oil terminated polymer and preparation method and application thereof Download PDFInfo
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- CN111018713A CN111018713A CN201911320901.8A CN201911320901A CN111018713A CN 111018713 A CN111018713 A CN 111018713A CN 201911320901 A CN201911320901 A CN 201911320901A CN 111018713 A CN111018713 A CN 111018713A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/66—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety
- C07C69/73—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of unsaturated acids
- C07C69/732—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of unsaturated acids of unsaturated hydroxy carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C3/00—Tanning; Compositions for tanning
- C14C3/02—Chemical tanning
- C14C3/08—Chemical tanning by organic agents
- C14C3/22—Chemical tanning by organic agents using polymerisation products
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- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C9/00—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes
- C14C9/02—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes using fatty or oily materials, e.g. fat liquoring
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Abstract
The invention discloses a pentaerythritol epoxy modified castor oil terminated polymer. It has a structure shown in the following formula I, wherein R is selected from C2‑10Alkoxy, n is a number in the range of 1-10. Mixing pentaerythritol and diethylene glycol dimethyl ether in an alkaline environment, heating until the materials are molten, performing vacuum dehydration, and adding an epoxy compound into the materials to react in an inert atmosphere; and after the reaction is carried out until the system pressure is stable, adjusting the pH value of the system after cooling, adding ricinoleic acid and a catalyst into the system, and obtaining the pentaerythritol epoxy modified castor oil terminated polymer after the reaction is finished. It can be used as leather fatting agent or retanning agent.
Description
Technical Field
The invention belongs to the field of leather additives, and particularly relates to a pentaerythritol epoxy modified castor oil terminated polymer, and a preparation method and application thereof.
Background
The greasing is a key process in the leather production, and the crust leather is greased reasonably and properly to absorb a proper amount of greasing materials, recover the original softness and elasticity of the crust leather, prevent the leather from being stiff and cracking and endow the leather with certain service performance. By the greasing, the tensile strength, the toughness, the elongation, the leather yield and the like of the leather are improved, and the leather has good hand feeling.
At present, the domestic fat-liquoring agent mostly takes a straight-chain anionic compound as a main component, the fat-liquoring agent is fixed in leather by combining a terminal carboxyl group, a hydroxyl group or an anionic group with chromium, the straight-chain fat-liquoring agent cannot form a three-dimensional structure and can only be combined with 1-2 chromium elements, the softness of the leather can be properly improved, the tensile strength and fullness of the leather are slightly improved, meanwhile, the fat-liquoring agent of an anionic material is easily influenced by water quality, for example, when the content of calcium and magnesium ions in water is high, the fat-liquoring agent is easy to break emulsion, so that oil stains are generated to cause floating oil on the surface of the leather, and the.
Disclosure of Invention
The invention aims to provide a pentaerythritol epoxy modified castor oil terminated polymer, and a preparation method and application thereof.
The invention provides a pentaerythritol epoxy modified castor oil terminated polymer, which has a structure shown as the following formula I:
wherein R is selected from C2-10Alkoxy radicals, e.g. C2-6Alkoxy radical, C2-4Alkoxy, preferably ethoxy or propoxy;
n ranges from 1 to 10, such as 1 to 5, 1 to 4, and 1 to 3; illustratively, the value may be 1, 1.5, 1.6, 2, 2.3, 2.5, or 3.
Preferably, the pentaerythritol epoxy modified castor oil terminated polymer has a structure as shown in formula II or formula III:
according to the technical scheme of the invention, the raw materials for preparing the pentaerythritol epoxy modified castor oil terminated polymer comprise: pentaerythritol, alkaline solution, diethylene glycol dimethyl ether, epoxy compound and ricinoleic acid. Further, the mass ratio of the pentaerythritol, the alkali solution, the diethylene glycol dimethyl ether, the epoxy compound and the ricinoleic acid is (0.5-4): 0.05-0.3): 0.1-2): 0.5-30): 5-25, preferably (1-2): 0.1-0.2): 0.5-1): 1-20): 5-20; illustratively, the mass ratio is 1:0.1:0.5:9.3:12, 1.4:0.12:0.5:9.4:10, 2:0.2:1:16.1: 15.
Wherein, the alkali solution can be potassium hydroxide aqueous solution or sodium hydroxide aqueous solution. Further, the alkali solution has a concentration of 30 to 40 wt%, such as 32 to 38 wt%, illustratively 30 wt%, 34 wt%, 38 wt%.
Further, the raw material can also comprise a catalyst, and the catalyst is selected from copper sulfate and SO4 2-/ZrO2、Al2O3/SiO2At least one of (1). Wherein the mass ratio of the catalyst to the pentaerythritol is (0.2-2): (0.5-4), preferably (0.7-1.2): (1-2); illustratively, the mass ratio is 0.8:1, 1.0:1.4, 0.5: 2.
Further, the present invention also provides a method for preparing the pentaerythritol epoxy modified castor oil terminated polymer, comprising the following steps:
(1) mixing pentaerythritol and diethylene glycol dimethyl ether in an alkaline environment, heating until the materials are molten, performing vacuum dehydration, and adding an epoxy compound into the materials to react in an inert atmosphere;
(2) and (2) after the reaction in the step (1) is carried out until the system pressure is stable, adjusting the pH value of the system after cooling, adding ricinoleic acid and a catalyst into the system, and obtaining the pentaerythritol epoxy modified castor oil terminated polymer after the reaction is finished.
According to an aspect of the present invention, in step (1), the alkaline environment may be provided by an alkaline solution, which has the meaning as described above.
According to the technical scheme of the invention, the pentaerythritol, the alkaline solution, the diethylene glycol dimethyl ether, the epoxy compound, the ricinoleic acid and the catalyst have the meanings and the mass ratio as described above.
According to the technical scheme of the invention, in the step (1), the dehydration temperature is 100-.
According to the technical scheme of the invention, in the step (1), the inert atmosphere is nitrogen, argon or helium, and preferably nitrogen.
According to the technical scheme of the invention, in the step (1), the temperature of the system when the epoxy compound is added is 130-170 ℃, for example 140-160 ℃, and exemplarily the temperature is 140 ℃, 150 ℃ and 160 ℃.
According to the technical scheme of the invention, in the step (1), the system pressure is controlled to be 0.2-0.5MPa, such as 0.3-0.4MPa during the reaction.
According to the technical scheme of the invention, in the step (1), the epoxy compound can be selected from ethylene oxide or propylene oxide. Wherein, when the epoxy compound is ethylene oxide, the mass ratio of the epoxy compound to the pentaerythritol is (0.5-20): (0.5-4), preferably (1-8): (1-2), and exemplarily, the mass ratio is 3: 1; when the epoxy compound is propylene oxide, the mass ratio of the epoxy compound to the pentaerythritol is (1-30): (0.5-4), preferably (2-10): (1-2), and exemplarily, the mass ratio is 4:1.4, 8: 2.
According to the technical scheme of the invention, in the step (2), the temperature is reduced to 45-65 ℃, preferably 50-60 ℃, for example, the temperature is 50 ℃, 55 ℃ or 60 ℃.
According to the technical scheme of the invention, in the step (2), the pH value of the system is 6-8.5, such as 6.5-8, and exemplarily, the pH value is 6, 6.5, 7 and 8. For example, the system pH is adjusted by adding acid; the acid may be glacial acetic acid or formic acid.
According to the technical scheme of the invention, in the step (2), the temperature of the reaction is 130-150 ℃, for example, 135-150 ℃, 140-145 ℃, exemplarily 135 ℃, 138 ℃, 140 ℃, 145 ℃. Further, the reaction time is 3 to 10 hours, such as 4 to 6 hours, illustratively 4 hours, 5 hours, 6 hours. Further, after the reaction is completed, vacuum is applied for incubation, for example, for 0.5 to 5 hours, preferably for 1 to 3 hours, and illustratively for 2 hours. Further, after the heat preservation is completed, the temperature is reduced, the mixture is kept still, the upper layer liquid is taken out, and the pH value of the liquid is adjusted to 6-8 (for example, 6.2-7.5, preferably 6.5-7), so that the product is obtained.
According to the solution of the present invention, in step (2), the catalyst has the meaning and the amount as described above.
According to an embodiment of the invention, the preparation method comprises the steps of:
putting 0.5-4 parts of pentaerythritol into a reaction kettle, adding 0.05-0.3 part of alkali solution, finally adding 0.1-2 parts of diethylene glycol dimethyl ether, heating to melt the materials, stirring, performing vacuum dehydration, heating to 110-120 ℃ for heat preservation until the dehydration is completed, performing air replacement by using nitrogen, heating to 140-160 ℃, introducing 0.5-20 parts of ethylene oxide or 1-30 parts of propylene oxide into the reaction kettle, controlling the pressure to be 0.3-0.4MPa, reacting until the pressure is stable, cooling to 50-60 ℃, adjusting the pH of the system to 6-8, adding a mixture of 5-20 parts of ricinoleic acid and 0.2-2 parts of catalyst into the reaction kettle, controlling the temperature to be 130-150 ℃, stirring for reaction for 4-6 hours, vacuumizing and preserving the heat, and after the heat preservation is finished, cooling to normal temperature, standing to enable the catalyst to be settled, taking the upper layer liquid, and adjusting the pH value of the product to 6-8 to obtain the pentaerythritol epoxy modified castor oil terminated polymer.
The invention also provides a pentaerythritol epoxy modified castor oil terminated polymer prepared by the method.
Further, the invention provides the application of the pentaerythritol epoxy modified castor oil terminated polymer as a leather auxiliary agent, preferably as a leather fatting agent or a leather retanning agent.
The inventor finds that: the pentaerythritol has the characteristic of high branching degree, the polyoxyethylene ether or polyoxypropylene ether synthesized by taking pentaerythritol as starting alcohol can adjust the softness and the hydrophile-lipophile degree of a product by adjusting the length of ethoxy or propoxy, and the leather assistant with different hydrophile-lipophile degrees and self-emulsifying capacity can be obtained after the castor oil acid is used for blocking the end of the product.
The invention has the beneficial effects that:
1. by using pentaerythritol as starting alcohol, dendritic leather auxiliary molecules with good dispersing capacity and self-emulsifying capacity are obtained, and the dendritic leather auxiliary molecules have a structure with multi-terminal active groups, can be combined with a plurality of collagen fibers of leather or tanning agents among the collagen fibers, are not easy to wash out by water and solvents, have good combining capacity, have good filling performance, can increase the softness and elasticity of the leather, and have high efficiency and multiple functions.
2. The preparation method and the product have the advantages of strong application practicability, reasonable and scientific preparation method, integrated innovation, environmental protection and low reagent residue in the preparation and application processes, the used organic solvent and catalyst can be recycled, and the modified natural oil end-capped epoxy ether compound has good biodegradability and is environment-friendly.
The polymer prepared by using ricinoleic acid as a main component and polyoxyethylene ether or polyoxypropylene ether as a secondary component has environmental protection performance, and after the polymer is applied to a fatliquoring or retanning process, the residual quantity in fatliquoring waste liquid and retanning waste liquid is small, and the residual polymer is easy to decompose and causes less pollution.
Definition and description of terms
Unless otherwise indicated, the definitions of groups and terms described in the specification and claims of the present application, including definitions thereof as examples, exemplary definitions, preferred definitions, definitions described in tables, definitions of specific compounds in the examples, and the like, may be arbitrarily combined and coupled with each other. The definitions of the groups and the structures of the compounds in such combinations and after the combination are within the scope of the present specification.
Where a range of numerical values is recited in the specification and claims of this application, and where the range is defined as "a number", it is understood that the two endpoints of the range and each number within the range are recited. For example, "a number of 1 to 10" is to be understood as describing not only each integer of 1, 2, 3, 4, 5, 6, 7, 8, 9 and 10 but also at least the sum of each integer and 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, respectively.
“C2-10Alkoxy "is understood to mean a straight-chain or branched saturated alkoxy group having 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10 carbon atoms. The alkoxy group is, for example, ethoxy, propoxy, butoxy, etc., or an isomer thereof.
Drawings
FIG. 1 shows the nuclear magnetic spectrum of a pentaerythritol epoxy modified castor oil terminated polymer obtained in example 1.
Detailed Description
The compounds of the general formula and the preparation and use thereof according to the present invention will be described in further detail with reference to the following examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Information on instruments used in examples and test examples:
| name of instrument | Manufacturer of the product | Model number |
| Tensile strength tester | Leather tensile strength tester | XK8014 |
| Tear strength tester | Leather tensile strength tester | XK8014 |
| Leather shrinkage temperature measuring instrument | Shanxi university of science and technology | MSW-YD4 type |
Example 1
Putting 1 part of pentaerythritol into a reaction kettle, adding 0.1 part of 30 wt% potassium hydroxide aqueous solution, finally adding 0.5 part of diethylene glycol dimethyl ether, heating until the materials are molten, then stirring is started, vacuum is started for dehydration, the temperature is raised to 110 ℃, the temperature is kept until the dehydration is finished, nitrogen is used for air replacement, then heating to 140 ℃, introducing 9.3 parts of ethylene oxide into the reaction kettle, controlling the pressure to be 0.3-0.4MPa, reacting until the pressure is stable, then cooling to 50-60 ℃, adjusting the pH to 6 by using glacial acetic acid, adding 12 parts of ricinoleic acid and 0.8 part of copper sulfate into a reaction kettle, controlling the temperature to be 135 ℃, stirring and reacting for 6 hours, then vacuumizing and preserving heat for 2h, cooling to normal temperature after heat preservation, standing to enable the catalyst to settle, taking the upper layer liquid, and adjusting the pH value of the product to 7 to obtain the pentaerythritol epoxy modified castor oil terminated polymer.
The reaction equation is as follows:
FIG. 1 shows the nuclear magnetic spectrum of the pentaerythritol epoxy modified castor oil terminated polymer prepared in this example: (1H NMR(300MHz,CDCl3) δ 5.45-5.25(m,8H),4.39-3.97(m,8H),3.81-3.41(m,48H),3.25-2.99(m,8H),2.39-2.21(m,12H),2.13-1.88(m,12H),1.72-1.51(m,8H),1.43-1.12(m,72H),0.98-0.75(m, 12H). It can be seen that the product of this example was successfully prepared.
Example 2
Putting 1.4 parts of pentaerythritol into a reaction kettle, adding 0.12 part of 34 wt% potassium hydroxide aqueous solution, finally adding 0.5 part of diethylene glycol dimethyl ether, heating until the materials are molten, starting stirring, starting vacuum to dehydrate, heating to 115 ℃, keeping the temperature until dehydration is completed, performing air replacement by using nitrogen, heating to 150 ℃, introducing 9.4 parts of propylene oxide into the reaction kettle, controlling the pressure to be 0.3-0.4MPa, reacting until the pressure is stable, cooling to 50-60 ℃, adjusting the pH to 6.5 by using glacial acetic acid, then adding 10 parts of ricinoleic acid and 1.0 part of SO4 2-/ZrO2Adding the mixture into a reaction kettle, controlling the temperature to be between 140 and 145 ℃, stirring and reacting for 5h, then vacuumizing and preserving heat for 2h, cooling to normal temperature after heat preservation is finished, standing to enable the catalyst to settle, taking the upper-layer liquid, and adjusting the pH value of the product to 6 to obtain the pentaerythritol epoxy modified castor oil terminated polymer.
The reaction equation is as follows:
example 3
Putting 2 parts of pentaerythritol into a reaction kettle, adding 0.2 part of 38 wt% potassium hydroxide aqueous solution, finally adding 1 part of diethylene glycol dimethyl ether, heating until the materials are molten, starting stirring, starting vacuum to dehydrate, heating to 120 ℃, keeping the temperature until dehydration is completed, performing air replacement by using nitrogen, heating to 160 ℃, introducing 16.1 parts of ethylene oxide into the reaction kettle, controlling the pressure to be 0.3-0.4MPa, reacting until the pressure is stable, cooling to 60 ℃, adjusting the pH to 8 by using glacial acetic acid, and then adding 15 parts of ricinoleic acid and 0.4 part of SO4 2-/ZrO20.5 part of Al2O3/SiO2The mixture is added into a reaction kettle, the temperature is controlled to be between 130 and 150 ℃, the stirring reaction is carried out for 5 hours, then the vacuum pumping and the heat preservation are carried out for 2 hours, after the heat preservation is finished, the temperature is reduced to the normal temperature, the standing is carried out to enable the catalyst to be settled, the upper liquid is taken, and the pH value of the product is adjusted to 7, thus obtaining the pentaerythritol epoxy modified castor oil terminated polymer.
The reaction equation is as follows:
test example 1
The leather is treated by the pentaerythritol epoxy modified castor oil terminated polymer prepared in the embodiment 1 of the invention, and the treatment method as the fatting agent comprises the following steps:
(1) putting the weighed blue leather into a rotary drum, taking the weight of the blue leather as a material basis, adding water with the same weight as the blue leather and sodium bicarbonate with the weight of 2.4 percent of the weight of the blue leather into the rotary drum, rotating the rotary drum for 60min at the temperature of 30 ℃, detecting the pH value of a system to be 6.0-6.5, and discharging liquid after the pH value is reached;
(2) adding water into the drum again, wherein the weight of the water is 2 times of that of the blue, rotating the drum for 10min at room temperature, and discharging the liquid after cleaning;
(3) after the step (2) is finished, adding water with the temperature of 50 ℃ and the amount of 4 times of the weight of the blue leather and the polymer obtained in the example 1 with the weight of 10% of the weight of the blue leather into a rotary drum, rotating for 60min, adding formic acid with the weight of 1.7% of the weight of the blue leather into the system, rotating for 10min, adding formic acid with the weight of 2.2% of the weight of the blue leather, rotating for 10min, detecting the end point pH value to be 3.2-3.6, taking out the drum, and drying the blue leather. The leather obtained from the treatment is designated sample 2.
The leather samples 1 and 2 were tested for their performance in the manner described above, using the leather samples obtained without the polymer treatment of example 1 as a blank (designated as sample 1), and the results of the performance tests are shown in Table 1.
TABLE 1
Remarking: the tearing strength is measured by GB T17928-1999 leather pinhole tearing strength measuring method; tensile Strength was measured using QB-T2710 and 2018, methods for measuring tensile Strength and elongation in physical and mechanical tests of leather.
Table 1 shows the effect of the pentaerythritol epoxy modified castor oil terminated polymer prepared in example 1 on the physical and mechanical properties of the leather after fatliquoring, and the results show that: after the polymer is used as a fatting agent for leather fatting operation, the tensile strength and the tear strength of the polymer are obviously improved, which indicates that the polymer has a crosslinking effect in the leather.
Test example 2
Leather was treated with the pentaerythritol epoxy modified castor oil capped polymer prepared in example 1 of the present invention as a retanning agent by the following method:
(1) putting the weighed blue leather into a rotary drum, adding water with the same weight as the blue leather into the rotary drum by taking the weight of the blue leather as a material basis, and rotating for 10min at 40 ℃;
(2) then adding the polymer prepared in the example 1, wherein the using amount of the polymer is 7 percent of the weight of the blue leather, and rotating for 180 min;
(3) and (3) after the step (2) is finished, adding sodium bicarbonate accounting for 1% of the weight of the blue leather into the system to adjust the pH value of the system, rotating for 15min, detecting the end point pH value of 4.0-4.2, and after the detection is finished, discharging the blue leather out of the drum.
The above procedure was followed for 3 batches of leather, the treated samples were designated # 4, # 5 and # 6, and the leather samples from the example 1 polymer treatment were not added as blanks (designated # 1, # 2 and # 3). For leather samples # 1-6 #
The shrinkage temperature of the leather was measured, and the results are shown in Table 2.
TABLE 2
Remarking: measurement of shrinkage temperature was carried out by QB/T2713-2005 "measurement method of shrinkage temperature in physical and mechanical test of leather".
Table 2 shows the effect of the pentaerythritol epoxy modified castor oil capped polymer prepared in example 1 on the shrinkage temperature Ts of the leather after retanning, which was observed to increase the shrinkage temperature of the leather after retanning by 4.3 ℃ on average. The results show that the polymer of the invention is combined with chrome tanning agent or leather collagen in leather, thereby generating cross linking effect and playing a role in strengthening tanning.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A pentaerythritol epoxy modified castor oil terminated polymer having the structure shown in formula i below:
wherein R is selected from C2-10Alkoxy, n is a number in the range of 1-10.
2. The polymer of claim 1, wherein R is selected from C2-6An alkoxy group;
preferably, n ranges from a number between 1 and 6.
3. The polymer of claim 1 or 2, wherein the polymer has a structure according to formula ii or formula iii:
4. the polymer of any of claims 1-3, wherein the starting materials for preparing the polymer comprise: pentaerythritol, alkaline solutions, diethylene glycol dimethyl ether, epoxy compounds and ricinoleic acid;
preferably, the mass ratio of the pentaerythritol to the alkali solution to the diethylene glycol dimethyl ether to the epoxy compound to the ricinoleic acid is (0.5-4): 0.05-0.3): 0.1-2: (0.5-30): 5-25);
preferably, the alkali solution is an aqueous potassium hydroxide solution or an aqueous sodium hydroxide solution;
preferably, the concentration of the alkali solution is 30-40 wt%;
preferably, the raw material further comprises a catalyst selected from copper sulfate and SO4 2-/ZrO2、Al2O3/SiO2At least one of;
preferably, the mass ratio of the catalyst to the pentaerythritol is (0.2-2) to (0.5-4).
5. A process for the preparation of a pentaerythritol epoxy modified castor oil capped polymer according to any of the claims 1 to 4, characterized in that it comprises the steps of:
(1) mixing pentaerythritol and diethylene glycol dimethyl ether in an alkaline environment, heating until the materials are molten, performing vacuum dehydration, and adding an epoxy compound into the materials to react in an inert atmosphere;
(2) and (2) after the reaction in the step (1) is carried out until the system pressure is stable, adjusting the pH value of the system after cooling, adding ricinoleic acid and a catalyst into the system, and obtaining the pentaerythritol epoxy modified castor oil terminated polymer after the reaction is finished.
6. The process according to claim 5, wherein in step (1), the alkaline environment is provided by an alkaline solution having the meaning as defined in claim 4;
preferably, the pentaerythritol, the alkali solution, the diglyme, the epoxy compound, the ricinoleic acid and the catalyst have the meaning and mass ratio as defined in claim 4.
7. The method according to claim 5 or 6, wherein in the step (1), the temperature of the dehydration is 100-130 ℃;
preferably, in step (1), the inert atmosphere is nitrogen, argon or helium;
preferably, in the step (1), the temperature of the system when the epoxy compound is added is 130-170 ℃;
preferably, in the step (1), the system pressure is controlled to be 0.2-0.5MPa during the reaction;
preferably, in step (1), the epoxide compound is selected from ethylene oxide or propylene oxide.
8. The method according to any one of claims 5 to 7, wherein in the step (2), the temperature is reduced to 45 to 65 ℃;
preferably, in the step (2), the pH value of the system is 6-8.5;
preferably, in the step (2), the reaction temperature is 130-150 ℃, and the reaction time is 3-10 h;
preferably, after the reaction is finished, vacuumizing and preserving heat;
preferably, after the heat preservation is finished, cooling, standing, taking the upper layer liquid, and adjusting the pH value of the liquid to 6-8 to obtain the product.
9. Pentaerythritol epoxy modified castor oil terminated polymer prepared according to any of claims 5 to 8.
10. Use of a polymer according to any of claims 1 to 4 and 9 as an aid to leather, preferably as a leather fatliquor or leather retanning agent.
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| CN111592648A (en) * | 2020-04-30 | 2020-08-28 | 佳化化学（茂名）有限公司 | Method for synthesizing pentaerythritol polyoxyethylene ether stearate |
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