CN113896818A - Emulsifier and PVB resin production method using same - Google Patents
Emulsifier and PVB resin production method using same Download PDFInfo
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Abstract
The invention discloses a multifunctional emulsifier and a PVB resin production method using the same, and belongs to the technical field of emulsifiers. The multifunctional emulsifier comprises a multifunctional assistant PVB-T1 and a multifunctional assistant PVB-T2, wherein the multifunctional assistant PVB-T1 comprises polyoxyethylene ether, and the multifunctional assistant PVB-T2 comprises isomeric polyol ether; the PVB resin production method using the emulsifier comprises the following steps: adding the multifunctional emulsifier into a PVA aqueous solution, uniformly stirring, adding butyraldehyde, performing catalytic polymerization to obtain PVB resin particles, rinsing and drying the PVB resin particles to obtain the PVB resin. The multifunctional emulsifier can greatly reduce the foaming amount in the PVB resin preparation process, the residual amount of the emulsifier in the finished PVB resin is extremely low, and the generation amount of defective products of the PVB resin outside the standard particle size range can be obviously reduced.
Description
Technical Field
The invention belongs to the technical field of emulsifiers, and particularly relates to an emulsifier and a PVB resin production method using the emulsifier.
Background
PVB resin is the most main raw material for manufacturing the automotive safety glass doubling, and the domestic production and sales volume keeps high-speed growth in recent years. At present, the production of PVB resin mainly adopts an emulsion polymerization process, butyraldehyde is prepared into emulsion by using an emulsifier, then the emulsion is subjected to condensation reaction with a raw material PVA, and a finished product is obtained after the generated PVB is washed and purified.
The emulsifier plays an important role in the synthesis of PVB resin, the emulsifier selected by the emulsion polymerization process of the PVB resin at present is conventional products such as OP-10, fast T50 and the like, the products have strong emulsifying capacity and low price and are widely used, but along with the increasing requirement of the market on the quality of the PVB resin, the defects caused by the conventional emulsifier are more and more obvious, and the PVB resin is mainly expressed in the following points:
(1) the conventional emulsifier is easy to foam, and a large amount of foam can reduce the effective utilization rate of containers such as a reaction kettle and the like, reduce the feeding materials and further influence the yield;
(2) the size of micelle particles formed by the emulsifier determines the particle size of PVB resin particles, and the size of micelles formed by the conventional emulsifier is not uniform, so that the particle size of the PVB resin particles is not uniform, and the quality of finished products is reduced;
(3) after the reaction is finished, the residual quantity of the conventional emulsifier on PVB resin particles is too much, so that the impurity content of the resin is increased, the white fog or blue light phenomenon appears on a film obtained by pressing the PVB particles, and the quality of the film is seriously influenced;
(4) the conventional emulsifier has insufficient hydrophilicity, needs a long and tedious rinsing process to remove, prolongs the production period, restricts the yield, and simultaneously has excessive energy consumption and water consumption, thereby not compounding the current green and environment-friendly production and operation concept of China.
The Chinese invention patent with the publication number of CN103007587B and the application date of 2012-11-28 discloses an emulsification defoaming system and a PVB resin production method adopting the system, and relates to an additive and application thereof in a resin production process, wherein the additive is formed by combining an emulsifier and a defoaming agent, the emulsifier accounts for 50-99.9% by weight, and the emulsifier is hexadecyl sodium sulfosuccinate or a mixture of octyl phenyl polyoxyethylene ether and sodium alkyl sulfosuccinate. The application of the emulsification defoaming system can eliminate foam generated by stirring on the premise of obtaining a good emulsification effect, thereby reducing the generation of massive waste materials and improving the quality and yield of products. Meanwhile, the defoaming agent applied in the emulsifying defoaming system is also beneficial to improving the compatibility of the plasticizer and the resin. Due to the existence of the defoaming agent, bubbles can be eliminated in the subsequent extrusion casting processing process of the resin, and the obtained film has no defect;
the Chinese invention patent with the publication number of CN103965382A and the application date of 2014-04-10 discloses a composite catalytic system and a PVB resin production method using the composite catalytic system, in the scheme, the catalytic system is formed by compounding and combining an emulsifier and a phase transfer catalyst, the mass ratio of the emulsifier to the phase transfer catalyst is 1-30: 1-70, and preferably the mass ratio of the emulsifier to the phase transfer catalyst is 1-8: 1 to 30. The composite catalytic system can promote the butyraldehyde dispersion in the PVB resin production process, effectively reduce the reactant viscosity in the condensation reaction of the PVA and the butyraldehyde, promote the precipitation of the PVB, improve the PVB reaction efficiency, improve the reaction uniformity and reduce material agglomeration. The PVB resin prepared by adopting the composite catalytic system has better butyraldehyde dispersion, lower reactant viscosity in the condensation reaction, more uniform reaction, capability of effectively reducing material agglomeration and improved product quality.
The above patents have their respective features, but none of them can reduce the generation of defective PVB resin particles while ensuring a substantial reduction in the amount of foaming.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems in the prior art, the invention provides the emulsifier and the PVB resin production method using the emulsifier, which can quickly and efficiently emulsify butyraldehyde into homogeneous emulsion to ensure that the butyraldehyde is fully contacted with PVA, thereby improving the conversion rate of polymerization reaction, ensuring that the foaming amount is greatly reduced, and reducing the generation amount of defective PVB resin particles.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
The multifunctional emulsifier comprises a multifunctional assistant PVB-T1 and a multifunctional assistant PVB-T2, wherein the multifunctional assistant PVB-T1 comprises polyoxyethylene ether, the multifunctional assistant PVB-T2 comprises isomeric polyol ether, and the mass percentage of the multifunctional assistant PVB-T1 to the multifunctional assistant PVB-T2 is 2: 1.
The invention also provides a PVB resin production method, which comprises the following steps:
adding a multifunctional emulsifier into a PVA aqueous solution, uniformly stirring, adding butyraldehyde, performing catalytic polymerization to obtain PVB resin particles, rinsing and drying the PVB resin particles to obtain PVB resin;
the multifunctional emulsifier is the multifunctional emulsifier as described in any one of the above items.
The preferable technical scheme is as follows:
in the preparation method of the multifunctional emulsifier, the mass fraction of the aqueous solution of PVA is 40-50%.
According to the preparation method of the multifunctional emulsifier, after the multifunctional emulsifier is added into the aqueous solution of PVA, the adding proportion of the multifunctional auxiliary PVB-T1 is 0.26% of the mass of the aqueous solution of PVA, and the adding proportion of the multifunctional auxiliary PVB-T2 is 0.13% of the mass of the aqueous solution of PVA.
According to the preparation method of the multifunctional emulsifier, the mass ratio of the added butyraldehyde to the PVA aqueous solution is 1: 1.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) compared with the traditional emulsifier, the novel emulsifier has the advantages that the foaming amount in the reaction process is greatly reduced, the equipment utilization rate is obviously improved, and the feeding amount of each reaction kettle can be improved by 20%;
(2) the multifunctional emulsifier is adopted to produce PVB resin, the particle size of the generated PVB resin particles is relatively uniform, and the generation amount of defective products outside the standard particle size range is reduced by 12%;
(3) the residual quantity of the multifunctional emulsifier in the finished PVB resin is extremely low, white fog and blue light phenomena basically disappear after the multifunctional emulsifier is pressed into a film, and the light transmittance of the film is improved by 15 percent;
(4) when the multifunctional emulsifier is used for producing PVB resin, the time consumption of each water-based process is reduced by 2-3 minutes, the 12 circulating water washing processes are saved by about 30 minutes in total, the daily yield can be improved by 7.8 tons, and meanwhile, the water consumption per day can be saved by 7.2 tons.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
The embodiment provides a multifunctional emulsifier, which comprises a multifunctional assistant PVB-T1 and a multifunctional assistant PVB-T2, wherein the multifunctional assistant PVB-T1 comprises polyoxyethylene ether, the multifunctional assistant PVB-T2 comprises isomeric polyol ether, and the mass percentage of the multifunctional assistant PVB-T1 to the multifunctional assistant PVB-T2 is 2: 1.
The composition and the amount of the multifunctional auxiliary agent PVB-T1 and the multifunctional auxiliary agent PVB-T2 in the composition range known to those skilled in the art can achieve the aim of the invention, but in order to better achieve the aim of the invention, the mass percentage of the multifunctional auxiliary agent PVB-T1 to the multifunctional auxiliary agent PVB-T2 is preferably 2: 1.
In the embodiment, the multifunctional auxiliary agent PVB-T1 mainly comprises polyoxyethylene ether and polyoxypropylene ether; the multifunctional auxiliary agent PVB-T1 mainly comprises polyoxyethylene ether and mixed polybasic ether.
More specifically, the polyoxyethylene ether may be ethylene oxide; the isomeric polyol ether may be a C9-C13 isomeric alcohol.
It is worth to be noted that, because the polyoxyethylene ether includes hydrophilic groups such as hydroxyl, ether bond, etc., and the heterogeneous polyol ether includes hydrophilic carbon chains and hydroxyl, in this embodiment, the multifunctional adjuvant PVB-T1 using the polyoxyethylene ether as a main component and the multifunctional adjuvant PVB-T2 using the heterogeneous polyol ether as a main component are both low-foaming substances, and the water solubility is excellent, so that the emulsifier can be fully dissolved in water and is not easy to foam; compared with the traditional emulsifier, the special component is compounded with the emulsifier, so that the steric hindrance between the generated resin particles can be increased, and the particles have good dispersibility.
For the multifunctional emulsifier in the embodiment, when the ratio between the multifunctional auxiliary agent PVB-T1 and the multifunctional auxiliary agent PVB-T2 is too high, the emulsifying capacity is excessive, and waste is caused; when the ratio of the multifunctional auxiliary agent PVB-T1 to the multifunctional auxiliary agent PVB-T2 is too low, the emulsifying capacity is insufficient, and butyraldehyde can not be completely emulsified.
It should be further noted that the multifunctional emulsifier in the present embodiment is mainly applied to the production process of PVB resin. The size of the micelle particles formed by the emulsifier determines the particle size of the PVB resin particles. In the conventional preparation process, the micelle formed by the conventional emulsifier is uneven in size, so that the particle size of PVB resin particles is uneven, and the quality of a finished product is reduced. In this embodiment, the size of the latex particles formed by the emulsifier is controlled within a narrow range by using a high-purity raw material and a precisely controlled production process, so as to ensure the uniformity of the particle size of the PVB resin particles.
In order to further ensure the dispersibility of the PVB resin particles in the production process of the PVB resin particles, the multifunctional emulsifier in this embodiment further includes antistatic groups such as hydroxyl groups and ether linkages, which are mainly used as antistatic components to make the surfaces of the PVB particles have the same charge, and the PVB resin particles are fully dispersed by electrostatic repulsion.
Although the multifunctional emulsifier provided by the embodiment is mainly used for the production process of PVB resin, the multifunctional emulsifier can also be applied to the production preparation process of other similar products and plays a positive and effective role.
Example 2
This example provides a method for producing PVB resin, which mainly comprises the following steps:
adding a multifunctional emulsifier into a PVA aqueous solution, uniformly stirring, adding butyraldehyde, performing catalytic polymerization to obtain PVB resin particles, rinsing and drying the PVB resin particles to obtain PVB resin;
the multifunctional emulsifier is the multifunctional emulsifier described in any one of embodiments 1-4.
It mainly comprises the following steps;
(1) preparing an aqueous solution of PVA;
PVA (polyvinyl alcohol) with the mass is added into 1L of purified water to be gathered, and the mass fraction of the prepared PVA water solution is 40-50%.
(2) Adding the multifunctional emulsifier into the aqueous solution of PVA;
after the multifunctional emulsifier is added into the aqueous solution of PVA, the adding proportion of the multifunctional auxiliary agent PVB-T1 is 0.26% of the mass of the aqueous solution of PVA, and the adding proportion of the multifunctional auxiliary agent PVB-T2 is 0.13% of the mass of the aqueous solution of PVA.
If the multifunctional emulsifier is added into the aqueous solution of the PVA, the adding proportion of the multifunctional auxiliary PVB-T1 is more than 0.26% of the mass of the aqueous solution of the PVA, and the adding proportion of the multifunctional auxiliary PVB-T2 is more than 0.13% of the mass of the aqueous solution of the PVA, so that the particle size of the produced latex is smaller, and the particle size of the PVB resin particles is smaller; if the multifunctional emulsifier is added into the aqueous solution of PVA, the adding proportion of the multifunctional auxiliary PVB-T1 is less than 0.26% of the mass of the aqueous solution of PVA, and the adding proportion of the multifunctional auxiliary PVB-T2 is less than 0.13% of the mass of the aqueous solution of PVA, so that the emulsifying capacity is insufficient, the butyraldehyde can not be fully dispersed in water, the reaction is incomplete, and the yield is reduced.
(3) Catalytic polymerization with butyraldehyde;
adding butyraldehyde into an aqueous solution of PVA containing a multifunctional emulsifier, wherein the mass ratio of the added butyraldehyde to the aqueous solution of PVA is 1:1, adjusting the pH value to 3-5, and keeping for 20-40 min to obtain a reaction mixture;
compared with the general PVB resin production process, the multifunctional emulsifier adopted in the embodiment is easier to rinse, so that the time consumption of each water-based process can be reduced by 2-3 minutes, the 12 circulating water washing processes can be saved by about 30 minutes in total, the daily yield can be improved by 7.8 tons, and meanwhile, the water consumption per day can be saved by 7.2 tons;
(4) rinsing and drying;
cooling the product obtained by the polymerization reaction to room temperature, centrifugally washing the product for 4 to 8 times by using a sodium hypochlorite solution, centrifugally washing the product for 1 to 3 times by using deionized water, centrifugally dehydrating the product, and drying the product in a drying chamber. Compared with the general PVB resin production process, the multifunctional emulsifier adopted in the embodiment is easier to rinse, so that the time consumption of each water-based process can be reduced by 2-3 minutes, 12 circulating water washing processes can be saved by about 30 minutes in total, the daily yield can be improved by 7.8 tons, meanwhile, the water consumption per day can be saved by 7.2 tons, the particle size of the latex formed by the emulsifier is relatively uniform, the particle size of the PVB resin particles generated in the embodiment is relatively uniform, and compared with the conventional PVB resin production process, the production of defective products outside the standard particle size range of the PVB resin is reduced by 12% by adopting the PVB resin production process in the embodiment.
It is worth to be noted that, the multifunctional emulsifier adopted in the embodiment has good self-defoaming property, which results in greatly reduced foaming amount in the reaction process, and greatly reduced foaming amount results in increased effective capacity of equipment, so that the utilization rate of the equipment is obviously improved, and the feeding amount of butyraldehyde in each reaction kettle can be increased by 20%.
Furthermore, the multifunctional emulsifier has good hydrophilicity and is easy to rinse, so that the residual quantity of the multifunctional emulsifier in finished PVB is extremely low, white fog and blue light phenomena basically disappear after the multifunctional emulsifier is pressed into a film, and the light transmittance of the film is improved by 15%.
Examples 3 to 5
According to the method of example 2, the prepared multifunctional emulsifier is applied to a conventional emulsion polymerization process of a PVB resin to prepare the PVB resin, the dosage of a multifunctional auxiliary agent PVB-T1 and the dosage of the multifunctional auxiliary agent PVB-T2 are counted, the hydrophilicity of the PVB resin is tested, the feeding amount of a reaction kettle in the emulsion polymerization process of the PVB resin and the amount of bubbles in the rinsing and drying processes are counted, the particle size uniformity and the generation amount of defective products of the finally prepared PVB resin are counted, and the phenomena of white fog and blue light are detected after film pressing, which is shown in the following table. The multifunctional auxiliary agent PVB-T1 comprises polyoxyethylene ether, and the multifunctional auxiliary agent PVB-T2 comprises isomeric polyol ether.
From examples 3 to 5, it can be seen that the emulsifier and the method for producing PVB resin using the emulsifier provided in example 1 can rapidly and efficiently emulsify butyraldehyde into a homogeneous emulsion, so that butyraldehyde can sufficiently contact PVA, thereby improving the conversion rate of polymerization reaction, and reducing the amount of generation of defective PVB resin particles while ensuring that the amount of foaming is greatly reduced.
The examples described herein are merely illustrative of the preferred embodiments of the present invention and do not limit the spirit and scope of the present invention, and various modifications and improvements made to the technical solutions of the present invention by those skilled in the art without departing from the design concept of the present invention shall fall within the protection scope of the present invention.
Claims (5)
1. A multifunctional emulsifier is characterized in that: the multifunctional auxiliary agent PVB-T1 and the multifunctional auxiliary agent PVB-T2 are included, wherein the multifunctional auxiliary agent PVB-T1 comprises polyoxyethylene ether, the multifunctional auxiliary agent PVB-T2 comprises isomeric polyol ether, and the mass percentage of the multifunctional auxiliary agent PVB-T1 to the multifunctional auxiliary agent PVB-T2 is 2: 1.
2. A PVB resin production method is characterized in that: adding a multifunctional emulsifier into a PVA aqueous solution, uniformly stirring, adding butyraldehyde, performing catalytic polymerization to obtain PVB resin particles, rinsing and drying the PVB resin particles to obtain PVB resin;
the multifunctional emulsifier is the multifunctional emulsifier of any one of claims 1 or 2.
3. A process for producing a PVB resin as claimed in claim 2 wherein the aqueous solution of PVA is present in an amount of 40% to 50% by weight.
4. A PVB resin production method according to claim 2, wherein the multifunctional emulsifier is added to the aqueous solution of PVA, the multifunctional auxiliary agent PVB-T1 is added in a proportion of 0.26% by mass of the aqueous solution of PVA, and the multifunctional auxiliary agent PVB-T2 is added in a proportion of 0.13% by mass of the aqueous solution of PVA.
5. A process for producing a PVB resin in accordance with claim 2 wherein the mass ratio of butyraldehyde added to the aqueous PVA solution is 1: 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115286727A (en) * | 2022-08-31 | 2022-11-04 | 中国科学院长春应用化学研究所 | Preparation method of low-residue polyvinyl butyral |
| CN116082540A (en) * | 2023-02-27 | 2023-05-09 | 江苏奥天利新材料有限公司 | Synthesis process of low-volatile odorless polyvinyl butyral resin powder |
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| US4725371A (en) * | 1985-01-29 | 1988-02-16 | Celanese Corporation | Partially oriented polyester yarn emulsion finish with elevated pH |
| CN103923725A (en) * | 2013-01-15 | 2014-07-16 | 中国石油化工股份有限公司 | Expanding oil composition |
| CN113563511A (en) * | 2021-09-23 | 2021-10-29 | 山东纳龙高科石油技术有限公司 | Preparation method of multifunctional integrated fracturing fluid |
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2021
- 2021-11-17 CN CN202111358846.9A patent/CN113896818A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4725371A (en) * | 1985-01-29 | 1988-02-16 | Celanese Corporation | Partially oriented polyester yarn emulsion finish with elevated pH |
| CN103923725A (en) * | 2013-01-15 | 2014-07-16 | 中国石油化工股份有限公司 | Expanding oil composition |
| CN113563511A (en) * | 2021-09-23 | 2021-10-29 | 山东纳龙高科石油技术有限公司 | Preparation method of multifunctional integrated fracturing fluid |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115286727A (en) * | 2022-08-31 | 2022-11-04 | 中国科学院长春应用化学研究所 | Preparation method of low-residue polyvinyl butyral |
| CN115286727B (en) * | 2022-08-31 | 2023-12-19 | 中国科学院长春应用化学研究所 | Preparation method of low-residue polyvinyl butyral |
| CN116082540A (en) * | 2023-02-27 | 2023-05-09 | 江苏奥天利新材料有限公司 | Synthesis process of low-volatile odorless polyvinyl butyral resin powder |
| CN116082540B (en) * | 2023-02-27 | 2023-09-26 | 江苏奥天利新材料有限公司 | Synthesis process of low-volatile odorless polyvinyl butyral resin powder |
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