CN112679720A - Preparation method of sorbitol-based polyether polyol and obtained polyether polyol - Google Patents
Preparation method of sorbitol-based polyether polyol and obtained polyether polyol Download PDFInfo
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Abstract
The invention provides a preparation method of sorbitol-based polyether polyol and the obtained polyether polyol, wherein solid sorbitol is used as an initiator, an alkali metal catalyst and an epoxy compound are added into a reaction system for more than two times, and the sorbitol-based polyether polyol is obtained through polymerization respectively and post-treatment. The invention reduces the viscosity of the initial reaction system by putting catalysts step by step for reaction, so that a product with high functionality can be made without adding solvents and functionality regulators, the product quality is controllable, the production period is short, the repeatability is strong, and the polyether with different molecular weights and properties can be produced to meet the requirements of different customers.
Description
Technical Field
The present invention relates to the preparation of polyether polyols, and in particular to the preparation of sorbitol-based polyether polyols.
Background
In the general polyether polyol category, polyether preparation by polymerization of ethylene glycol, propylene glycol, glycerin, hexanetriol, pentaerythritol, xylitol and sucrose as initiators with epoxides has been reported, and these polyether products can be used for various applications of soft, semi-soft and rigid foams. However, the industrial application of sorbitol as an initiator has been reported rarely, because the previous domestic sorbitol product is almost all 70% aqueous solution, and is difficult to be used as an initiator due to the high water content, and although solid sorbitol appears after the subsequent process improvement, the domestic research on the sorbitol is still less.
Solid sorbitol is used as a high-functionality initiator, and after sorbitol-based polyether is synthesized, foam plastic prepared from the sorbitol-based polyether is superior to traditional glyceryl polyether, xylitol-based polyether and sucrose-based polyether in the aspects of aging performance, dimensional stability, mechanical performance, softening temperature, oil resistance and the like.
The general preparation process of the sorbitol polyether at present is as follows: solid sorbitol is used as an initiator, alkali metal is used as a catalyst, and the solid sorbitol and epoxide are subjected to polymerization reaction at a certain temperature and under a certain pressure to generate crude sorbitol polyether. However, in order to lower the viscosity of the initial reaction system, it is common practice to add a solvent or a functionality modifier to the reaction vessel in advance to lower the viscosity of the initial reaction system. The addition of the solvent not only introduces impurities, but also needs to remove the impurities in the subsequent process of the reaction, which not only increases the reaction procedures, but also influences the quality of the final product due to unclean solvent removal. The addition of the functionality regulator can participate in polymerization reaction, so that the final functionality of the sorbitol polyether is reduced, and the final use performance of the product is influenced.
Chinese patent CN102617848A discloses a method for preparing sorbitol polyether polyol, wherein a modifier is added during the preparation process to improve the fluidity of sorbitol polyether polyol, but the corresponding product functionality is also reduced, which may have a certain influence on the mechanical properties of the foam product.
Chinese patent CN106146823A describes a three-stage preparation method of sorbitol polyether, which is to mix solid sorbitol and alkali metal catalyst and then directly react with epoxide at reaction temperature, but this method can increase system viscosity and make stirring difficult due to alkoxide generated by reaction of sorbitol and alkali metal catalyst, and subsequently it is not easy to remove by-product water completely, resulting in functionality slightly lower than 6, and because of stirring difficulty, the contact area between propylene oxide and alkoxide at the first stage is small, and it is difficult to react, and the production cycle of the whole production process is increased.
Therefore, by developing a new sorbitol-based polyether preparation process, the viscosity of the system can be reduced without adding a solvent or a regulator at the initial stage of the reaction, and a product with high functionality can be prepared, so that the preparation method has high economic value.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention discloses a novel preparation method of sorbitol-based polyether, which can prepare a product with high functionality without adding a solvent or a regulator to reduce the viscosity of the system at the initial stage of reaction, and has higher economic value.
One of the objects of the present invention is to provide a method for preparing sorbitol-based polyether polyol, wherein solid sorbitol is used as an initiator, an alkali metal catalyst and an epoxy compound are added into a reaction system for two or more times, and the obtained products are polymerized respectively to obtain the sorbitol-based polyether polyol. In the preparation method of the invention, no solvent or regulator is added in the preparation particularly in the initial stage.
In a preferred embodiment, the preparation method comprises the following steps:
step 1, taking solid sorbitol as an initiator, and carrying out first-stage polymerization on part of alkali metal catalyst and part of epoxy compound;
step 2, adding the rest alkali metal catalyst and the rest epoxy compound to carry out second-stage polymerization, and then removing the unreacted epoxy compound to obtain a sorbitol-based polyether polyol crude product;
and 3, carrying out post-treatment on the sorbitol-based polyether polyol crude product to obtain the sorbitol-based polyether polyol product.
In a preferred embodiment, in step 1, the solid sorbitol and a part of the alkali metal catalyst are placed in a reaction system, then the protection gas replacement is carried out, the temperature is raised to 110-150 ℃, and then the temperature is lowered to 80-130 ℃ for the first-stage polymerization.
Wherein the purpose of the temperature rise is to achieve dissolution and dehydration. The shielding gas comprises nitrogen and/or an inert gas, preferably nitrogen and/or argon.
In a preferred embodiment, in step 1, the amount of the partial alkali metal catalyst is 0.1 to 2%, preferably 0.2 to 1.5%, based on 100 wt% of the solid sorbitol.
In a further preferred embodiment, in step 1, the amount of the partial epoxy compound is 0.1 to 1.5 times, preferably 0.25 to 1 time, that of the solid sorbitol.
In a preferred embodiment, in step 2, the residual alkali metal catalyst is added into the reaction system, then the protective gas replacement is carried out, the temperature is raised to 110-150 ℃, and then the temperature is lowered to 80-130 ℃ for the second-stage polymerization.
Wherein the purpose of the temperature rise is to achieve dissolution and dehydration. The shielding gas comprises nitrogen and/or an inert gas, preferably selected from nitrogen and/or argon.
In a preferred embodiment, in step 2, the amount of the remaining alkali metal based catalyst in step 2 is 2% to 20%, preferably 3% to 15%, based on 100% by weight of the solid sorbitol.
In the second stage polymerization, the amount of the epoxy compound monomer added can be controlled by itself according to the molecular weight and properties of the desired product.
In a preferred embodiment, the ratio of the amount of the partial alkali metal catalyst used in the first stage polymerization in step 1 to the amount of the remaining alkali metal catalyst used in the second stage polymerization in step 2 is 1 (5-10), preferably 1: (6-8).
In the present invention, the catalyst added in the first stage polymerization is much less than the catalyst added in the second stage polymerization, which would otherwise result in a higher system viscosity.
In a preferred embodiment, the post-treatment of step 3 comprises sequentially emulsifying, neutralizing, adsorbing, dehydrating and filtering.
In a further preferred embodiment, the post-treatment of step 3 is carried out as follows:
(I) adding water into the crude sorbitol polyether for emulsification;
(II) adding oxalic acid or phosphoric acid, and neutralizing until the pH value is 4.5-6;
(III) adding an adsorbent to perform adsorption, wherein the adsorbent is preferably selected from one or more of magnesium silicate, aluminum silicate and magnesium aluminum silicate;
(IV) dehydrating and filtering to obtain the sorbitol-based polyether polyol product.
In a further preferred embodiment, in step (III), the adsorbent is dosed in an amount of crude sorbitol based polyether polyol (0.1-0.4) wt%.
In the prior art, solid sorbitol reacts with epoxide under the action of alkali metal catalyst mainly has three paths: one is a direct one-step reaction, but the reaction is difficult due to the high viscosity of the system in the initial stage of the reaction, the production period is long, and the indexes of each production batch are unstable. The second method is to add a solvent into the reaction system to reduce the viscosity of the initial system of the reaction, but a solvent removal procedure is required to be added subsequently, which affects the production cycle. The third method is to add a functionality regulator into the reaction system to reduce the viscosity of the initial system, but the regulator will participate in the reaction and affect the final functionality of the final product.
In the initial polymerization process, a little alkali metal catalyst is added firstly, so that the alkoxide amount generated in the initial reaction system is less, the viscosity of the system is much lower than that of the completely added alkali metal catalyst, the contact area between the initial reaction system and epoxy compound alkane in the first-stage polymerization is favorably increased, the reaction speed is improved, after the epoxy compound in the first-stage polymerization is polymerized, the viscosity of the whole polymerization system is greatly reduced due to the addition of the epoxy compound, the rest alkali metal catalyst is added at the moment, the viscosity of the system is increased, but the influence on the reaction speed of the subsequent epoxy compound is little.
The second object of the present invention is to provide a sorbitol-based polyether polyol obtained by the preparation method described in the first object of the present invention.
In a preferred embodiment, the sorbitol-based polyether polyol has a number average molecular weight of 500-12000g/mol, a moisture content of 0.1% or less and a pH of 5-7.
Compared with the prior art, the invention has the following beneficial effects: the invention reduces the viscosity of the initial reaction system by putting catalysts step by step for reaction, so that a product with high functionality can be made without adding solvents and functionality regulators, the product quality is controllable, the production period is short, the repeatability is strong, and the polyether with different molecular weights and properties can be produced to meet the requirements of different customers.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The raw materials used in the examples and comparative examples are disclosed in the prior art if not particularly limited, and may be, for example, directly purchased or prepared according to the preparation methods disclosed in the prior art.
In the examples and comparative examples, the average functionality was calculated from the formulation of the charge, the total sorbitol added as the initiator was 6, the number average molecular weight and the molecular weight distribution index were determined by GPC, the hydroxyl value was determined by acylation with phthalic anhydride (i.e., the hydroxyl value of the polyether polyol was determined by the acylation method), and the viscosity was determined by a rotational viscometer.
[ example 1 ]
Adding 200g of solid sorbitol and 1g of potassium hydroxide into a 2L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to 120 ℃, dehydrating, cooling to 90 ℃, starting to add 100g of propylene oxide, adding 6g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 120 ℃, dehydrating, cooling to 90 ℃, starting to add 1000g of propylene oxide, discharging after dropping until the pressure is stable, and obtaining the crude sorbitol polyether.
Putting the prepared crude sorbitol polyether into a refining kettle, adding 65g of pure water, stirring and emulsifying, heating to 90 ℃, adding 21g of phosphoric acid with the content of 50% for neutralization reaction after 1 hour, adding 3g of magnesium aluminum silicate for adsorption after 1 hour, dehydrating and filtering to obtain a finished product of sorbitol polyether, wherein the molecular weight is 443.6, the functionality is 6 and the hydroxyl value is 758.7 mgKOH/g.
[ example 2 ]
Adding 200g of solid sorbitol and 1g of potassium hydroxide into a 2L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to 120 ℃, dehydrating, cooling to 90 ℃, starting to add 100g of propylene oxide, adding 7g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 120 ℃, dehydrating, cooling to 90 ℃, starting to add 1200g of propylene oxide, discharging after dropping until the pressure is stable, and obtaining the crude sorbitol polyether.
Putting the prepared crude sorbitol polyether into a refining kettle, adding 75g of pure water, stirring and emulsifying, heating to 90 ℃, adding 24g of phosphoric acid with the content of 50% for neutralization reaction after 1 hour, adding 4g of magnesium aluminum silicate for adsorption after 1 hour, dehydrating and filtering to obtain a finished product of sorbitol polyether, wherein the molecular weight is 508.9, the functionality is 6 and the hydroxyl value is 661.4 mgKOH/g.
[ example 3 ]
Adding 200g of solid sorbitol and 1g of potassium hydroxide into a 2L stainless steel kettle, performing nitrogen replacement, stirring and heating to dissolve after the oxygen content in the kettle is measured to be less than 150ppm, dehydrating after the temperature is 120 ℃, cooling to 90 ℃, starting to add 100g of propylene oxide, adding 8g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 120 ℃, dehydrating after the temperature is reduced to 90 ℃, starting to add 1400g of a mixture of propylene oxide and ethylene oxide, wherein the ratio of the mixture to the propylene oxide to the ethylene oxide is 9:1, and discharging after dropping until the pressure is stable to obtain the crude sorbitol polyether.
Putting the prepared crude sorbitol polyether into a refining kettle, adding 85g of pure water, stirring and emulsifying, heating to 90 ℃, adding 27g of phosphoric acid with the content of 50% for neutralization reaction after 1 hour, adding 6g of magnesium aluminum silicate for adsorption after 1 hour, dehydrating and filtering to obtain a finished product of sorbitol polyether, wherein the molecular weight is 573.2, the functionality is 6 and the hydroxyl value is 587.2 mgKOH/g.
[ example 4 ]
Adding 200g of solid sorbitol and 0.6g of potassium hydroxide into a 2L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to 110 ℃, dehydrating, cooling to 80 ℃, starting to add 50g of propylene oxide, adding 4g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 110 ℃, dehydrating, cooling to 80 ℃, starting to add 530g of propylene oxide, discharging after dropping until the pressure is stable, and obtaining the crude sorbitol polyether.
The sorbitol polyether product was obtained by the same refining procedure as described in example 3.
[ example 5 ]
Adding 200g of solid sorbitol and 0.7g of potassium hydroxide into a 2L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to 130 ℃, dehydrating, cooling to 100 ℃, starting to add 100g of propylene oxide, adding 6.6g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 130 ℃, dehydrating, cooling to 100 ℃, starting to add 1000g of propylene oxide, discharging after dropping until the pressure is stable, and obtaining the crude sorbitol polyether.
Putting the prepared crude sorbitol polyether into a refining kettle, adding 65g of pure water, stirring and emulsifying, heating to 90 ℃, adding 21g of phosphoric acid with the content of 50% for neutralization reaction after 1 hour, adding 3g of magnesium aluminum silicate for adsorption after 1 hour, dehydrating and filtering to obtain a sorbitol polyether finished product with the molecular weight of 442.8, the functionality of 6 and the hydroxyl value of 760.2 mgKOH/g.
[ example 6 ]
Adding 200g of solid sorbitol and 2.5g of potassium hydroxide into a 3L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to 140 ℃, dehydrating, cooling to 110 ℃, starting to add 200g of propylene oxide, adding 20g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 140 ℃, dehydrating, cooling to 110 ℃, starting to add 1500g of propylene oxide, discharging after dropping until the pressure is stable, and obtaining the crude sorbitol polyether.
Putting the prepared crude sorbitol polyether into a refining kettle, adding 85g of pure water, stirring and emulsifying, heating to 90 ℃, adding 36g of phosphoric acid with the content of 50% for neutralization reaction after 1 hour, adding 7g of magnesium aluminum silicate for adsorption after 1 hour, dehydrating and filtering to obtain a finished product of sorbitol polyether, wherein the molecular weight is 575.3, the functionality is 6 and the hydroxyl value is 585.1 mgKOH/g.
[ example 7 ]
Adding 200g of solid sorbitol and 3g of potassium hydroxide into a 3L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to 130 ℃, dehydrating, cooling to 100 ℃, starting to add 250g of propylene oxide, adding 20g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 130 ℃, dehydrating, cooling to 100 ℃, starting to add 1500g of propylene oxide, discharging after dropping until the pressure is stable, and obtaining the crude sorbitol polyether.
Refining to obtain the sorbitol polyether finished product.
During the polymerization process, particularly at the initial stage of polymerization, the phenomena of influence on stirring and reaction progress caused by too high system viscosity do not occur.
In examples 1 to 7, there was no phenomenon that the stirring was affected and the reaction progress was affected by the viscosity of the system during the polymerization process, particularly at the initial stage of the polymerization.
Comparative example 1
200g of solid sorbitol and 7g of potassium hydroxide are added into a 2L stainless steel kettle, nitrogen replacement is carried out, after the oxygen content in the kettle is measured to be less than 150ppm, stirring is carried out, the temperature is raised for dissolution, dehydration is carried out after the temperature is 120 ℃, the temperature is reduced to 90 ℃, 1100g of propylene oxide is added, and the reaction is carried out.
The preparation process of the comparative example 1 can cause the viscosity of the system to be increased, the stirring is difficult, the byproduct water is difficult to completely dehydrate subsequently, the functionality is slightly lower than 6, the contact area of the propylene oxide and the alkoxide at the first section is small due to the stirring difficulty, the reaction is difficult, and the production period of the whole production procedure is prolonged.
Comparative example 2
Adding 200g of solid sorbitol and 7g of potassium hydroxide into a 2L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to dissolve, dehydrating after 120 ℃, cooling to 90 ℃, starting to add 100g of propylene oxide, adding 1000g of propylene oxide after dropping internal pressure until pressure is stable, and reacting.
In this comparative example 2, since no staged catalyst addition (even staged epoxy addition) was made, similar phenomena to those in comparative example 1 were observed in the preparation process, specifically, increased system viscosity, difficulty in stirring, and the like.
Comparative example 3
Adding 200g of solid sorbitol and 5g of potassium hydroxide into a 2L stainless steel kettle, performing nitrogen replacement, measuring the oxygen content in the kettle to be less than 150ppm, stirring, heating to 120 ℃, dehydrating, cooling to 90 ℃, starting to add 100g of propylene oxide, adding 2g of potassium hydroxide into the kettle after dropping until the pressure is stable, performing nitrogen replacement, heating to 120 ℃, dehydrating, cooling to 90 ℃, starting to add 1000g of propylene oxide, and reacting.
In this comparative example 3, since the amount of the catalyst added in the first-stage polymerization was too large, the viscosity increased and stirring became difficult in the system without adding the solvent and the modifier at the initial stage of the reaction.
Claims (10)
1. A preparation method of sorbitol-based polyether polyol is characterized in that solid sorbitol is used as an initiator, an alkali metal catalyst and an epoxy compound are added into a reaction system for more than two times, and the sorbitol-based polyether polyol is obtained after polymerization respectively.
2. The method of claim 1, comprising the steps of:
step 1, taking solid sorbitol as an initiator, and carrying out first-stage polymerization on part of alkali metal catalyst and part of epoxy compound;
step 2, adding the rest alkali metal catalyst and the rest epoxy compound to carry out second-stage polymerization, and then removing the unreacted epoxy compound to obtain a sorbitol-based polyether polyol crude product;
and 3, carrying out post-treatment on the sorbitol-based polyether polyol crude product to obtain the sorbitol-based polyether polyol product.
3. The preparation method according to claim 2, wherein in the step 1, the solid sorbitol and part of the alkali metal catalyst are placed in a reaction system, then the protection gas replacement is carried out, the temperature is raised to 110-150 ℃, and then the temperature is lowered to 80-130 ℃ for the first-stage polymerization.
4. The production method according to claim 2, wherein, in step 1,
the amount of the partial alkali metal catalyst is 0.1 to 2 percent, preferably 0.2 to 1.5 percent, based on 100 weight percent of the solid sorbitol.
5. The method according to claim 2, wherein the amount of the partial epoxy compound used in step 1 is 0.1 to 1.5 times, preferably 0.25 to 1 time, that of the solid sorbitol.
6. The preparation method according to claim 2, wherein in the step 2, the remaining alkali metal catalyst is added to the reaction system, then the replacement with the shielding gas is performed, the temperature is raised to 110 to 150 ℃, and then the temperature is lowered to 80 to 130 ℃ to perform the second-stage polymerization.
7. The method according to claim 2, wherein the amount of the remaining alkali metal-based catalyst in step 2 is 2 to 20%, preferably 3 to 15%, based on 100 wt% of the solid sorbitol in step 2.
8. The preparation method according to any one of claims 2 to 7, wherein the post-treatment in step 3 comprises emulsification, neutralization, adsorption, dehydration and filtration in sequence; preferably, the first and second electrodes are formed of a metal,
the post-treatment in step 3 is carried out as follows:
(I) adding water into the crude sorbitol polyether for emulsification;
(II) adding oxalic acid or phosphoric acid, and neutralizing until the pH value is 4.5-6;
(III) adding an adsorbent for adsorption;
(IV) dehydrating and filtering to obtain the sorbitol-based polyether polyol product.
9. The preparation method according to claim 8, wherein in the step (III), the adsorbent is selected from one or more of magnesium silicate, aluminum silicate and magnesium aluminum silicate, and preferably, the input amount of the adsorbent is 0.1-0.4 wt% of the crude sorbitol polyether polyol.
10. A sorbitol-based polyether polyol obtained by the preparation method of any one of claims 1 to 9; preferably, the number average molecular weight is 500-.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113667111A (en) * | 2021-08-31 | 2021-11-19 | 山东一诺威新材料有限公司 | Preparation method of sorbitol-based high molecular weight polyether polyol |
| CN114149578A (en) * | 2021-12-29 | 2022-03-08 | 滨化集团股份有限公司 | Method for removing potassium and sodium ions in polyether polyol |
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| EP0047371A1 (en) * | 1980-08-14 | 1982-03-17 | BASF Aktiengesellschaft | Method of preparing highly reactive poly(oxyalkylene-oxyethylene) ethers that contain hydroxyl groups |
| CN106008953A (en) * | 2016-08-01 | 2016-10-12 | 山东诺威新材料有限公司 | Preparation method of low unsaturation degree and high intersolubility high molecular weight polyether polyol |
| CN106146823A (en) * | 2016-07-30 | 2016-11-23 | 淄博德信联邦化学工业有限公司 | The preparation method of pure crystalline sorbitol polyether polyol |
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| EP0047371A1 (en) * | 1980-08-14 | 1982-03-17 | BASF Aktiengesellschaft | Method of preparing highly reactive poly(oxyalkylene-oxyethylene) ethers that contain hydroxyl groups |
| CN106146823A (en) * | 2016-07-30 | 2016-11-23 | 淄博德信联邦化学工业有限公司 | The preparation method of pure crystalline sorbitol polyether polyol |
| CN106008953A (en) * | 2016-08-01 | 2016-10-12 | 山东诺威新材料有限公司 | Preparation method of low unsaturation degree and high intersolubility high molecular weight polyether polyol |
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| CN113667111A (en) * | 2021-08-31 | 2021-11-19 | 山东一诺威新材料有限公司 | Preparation method of sorbitol-based high molecular weight polyether polyol |
| CN114149578A (en) * | 2021-12-29 | 2022-03-08 | 滨化集团股份有限公司 | Method for removing potassium and sodium ions in polyether polyol |
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