CN105713118A - Production method capable of reducing water discharge in PVB resin production - Google Patents
Production method capable of reducing water discharge in PVB resin production Download PDFInfo
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- CN105713118A CN105713118A CN201610260926.3A CN201610260926A CN105713118A CN 105713118 A CN105713118 A CN 105713118A CN 201610260926 A CN201610260926 A CN 201610260926A CN 105713118 A CN105713118 A CN 105713118A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/28—Condensation with aldehydes or ketones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/06—Treatment of polymer solutions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/06—Treatment of polymer solutions
- C08F6/12—Separation of polymers from solutions
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Abstract
The invention relates to a production method capable of reducing the water discharge in PVB production. The production method comprises the following steps: (1) dissolution; (2) filtration; (3) reaction; (4) stabilization; (5) heat preservation; (6) water washing; (7) acid washing; (8) addition of alkali to neutralize hydrochloric acid; (9) alkali washing; (10) wastewater recovery; (11) spin-drying; (12) wastewater recovery; and (13) acquisition of a finished product. In the invention, after the wastewater of the alkali washing and spin-drying processes is recycled, the water consumption of PVB resin production is reduced to about 38 tons, so that the production cost of PVB resin is lowered, the sewage discharge in PVB resin production is reduced, the use cost is lowered, and an environmental protection effect is realized.
Description
Technical field:
The present invention relates to a kind of production method reducing and producing PVB resin displacement.
Background technology:
Polyvinyl butyral resin Project Product belongs to thermoplastic macromolecule material field, is the main production raw material of polyvinyl butyral resin (PVB) glued membrane.By PVB resin powder through specialty plasticiser plasticising, then pass through double screw extruder extruded for PVB glued membrane.PVB glued membrane is with its excellent optical property, high temperature resistant, low temperature, mechanical performance and the adhesive property that unorganic glass is good becomes the necessary raw material producing all kinds of safety glasses.When being subject to extraneous intense impact, PVB glued membrane can apparatus with shock absorbing, do not produce flinders, while there is security feature, also have excellent sound insulation, light-operated, insulation, the performance such as heat insulation, antifog, be ideal safety glass rapidoprint.
The production of external PVB is concentrated mainly on the U.S., Japan and West Europe, and oneself reaches more than 130,000 tons to estimate total productive capacity.The U.S. is that PVB produces and consumes maximum country, main manufacturer You Shou promise company (branch company of SOLUTION, MANSANTO group), E.I.Du Pont Company and union carbide corporation.Shou Nuo company is PVB manufacturer maximum in the world, accounts for the 50% of whole world PVB production capacity, and the product of the said firm had both been used for producing diaphragm, again for priming paint, coating, the industry such as electric.The product of E.I.Du Pont Company is all almost that viscosity PVB resin is used for producing diaphragm, PVB film market, the world is divided equally with the SEKISUI (hydrops company) of Shou Nuo company, Japan, there are oneself independent raw material processing enterprise in three companies, take strict secrecy provision for the resin required for pvb film, plasticizer and processing technique.
The development of China PVB, from 1956, has been carried out the lab scale development work of vinyl acetate and acetal product thereof by Shenyang Chemical Engineering Inst and Tianjin synthetic material institute.The first designing institute of the Ministry of Chemical Industry in 1958 is that Jinxi Chemical Research Institute devises China tentative acetal workshop the earliest.Organic factory of Jinxi chemical industrial company is transferred in acetal workshop by Jinxi Chemical Research Institute in 1961, and PVB workshop, chemical plant, Jinxi in 1964 starts trial production.After the seventies, owing to PVB achieves breakthrough in the application of ceramic marble paper and aluminium-foil paper industry, thus having promoted the development of PVB industry.1985-1988, former China National Light Industrial Products Department takes the lead, tissue chemical plant, Jinxi, icy mountain peak chemical plant, Tianjin, Guizhou organic chemical industry's pilot plant, Shanghai optical research etc. domestic strong producer held PVB film decisive battle, want to realize the production domesticization of safety glass PVB film early, but not success because of various reasons, only Guizhou organic chemical industry pilot plant, Shanghai optical research are produced, but yield is relatively low, and quality cannot be competed with imported product.
The high-end PVB of China all relies on import, main cause is production technology and supporting insufficient raw material, due to PVB production technology be PVA (polyvinyl alcohol) aqueous solution under the effect of catalyst with polyvinyl butyral resin, dry after washing become PVB powder end resin.Comparing external production technology, our equipment and technology seriously falls behind external colleague.And China adopts is traditional old Technology, manufacturing enterprise does not have supporting PVB film research institution, and this is also cause the high terminal membrane PVB reason all relying on import.
Traditional PVB production technology water consumption is too high, and ton consumes about 100 tons, and not only not environmentally, and production cost is also high.
Summary of the invention:
It is an object of the invention to provide a kind of economy, the additive of environmental protection and utilize it to reduce the production method producing PVB resin displacement.
The present invention is achieved in that
A kind of production method reducing production PVB resin displacement, comprises the steps:
(1) dissolve: PVA is put in dissolution kettle and dissolves, PVA is dissolved into the PVA aqueous solution that concentration is 9～11%；
(2) filter: PVA aqueous solution step (1) dissolved and cold pure water plate type heat exchanger carry out heat exchange cooling；
(3) reaction: step (2) is put in reactor through the PVA aqueous solution of cooling, when PVA aqueous solution is heated to 15～20 DEG C by reactor, put into butyraldehyde, hydrochloric acid, PVA aqueous solution and butyraldehyde, hydrochloric acid react in a kettle., are put to calm still by reactant after reacting 0.5～1.5 hour；
(4) calm: step (3) reacted reactant to be heated up in calm still, within 1～5 hour, is warming up to 65～75 DEG C；
(5) insulation: after the reactant of step (4) is carried out insulation 0.5～1.5 hour in calm still, reactant is put to washing kettle；
(6) washing: by the reactant of step (5) with recycling water washing more than 5 times, specifically: first draining is to washing kettle fixed position, then mend and recycle water to graduation mark place in washing kettle, after stirring 15～25 minutes, draining is to sewage disposal, repeats above-mentioned action more than 5 times；
(7) acid is washed: by the reactant deionized water wash more than 2 times of step (6), specifically: first draining is to washing kettle fixed position, then mending deionized water to graduation mark place in washing kettle, after stirring 15～25 minutes, draining is to sewage disposal, repeats above-mentioned action more than 2 times；
(8) add in alkali and hydrochloric acid: in the reactant of step (7), add alkali liquor be neutralized reaction so that it is pH value reaches 11～13, and keeps more than 2 hours；
(9) soda: the water in the reactant of step (8) is discharged to recovery pond, then deionized water is mended to washing kettle graduation mark place, again in water discharge to recovery pond, soda action will be repeated until the water conductivity of reactant is less than 50 in washing kettle after stirring 15～25 minutes；
(10) waste water reclamation: by step (9) soda produce waste water reclaim, waste water is drained in waste water reclamation pond, the waste water of recovery for next time wash acid operation；
(11) drying is dried: be evacuated in drier by the reactant of step (10) and carry out drying operation；
(12) waste water reclamation: by step (11) dry dry produce waste water reclaim, waste water is drained in waste water reclamation pond, the waste water of recovery for next time wash acid operation；
(13) finished product: obtain PVB resin powder.
In above-mentioned a kind of production method reducing production PVB resin displacement, described resin: butyraldehyde: the weight ratio of hydrochloric acid=(14～16): (8～10): (2～3).
In above-mentioned a kind of production method reducing production PVB resin displacement, being additionally added additive in step (3) and promote the reaction of PVA and butyraldehyde, described additive is: the mixture of the sulfonate of emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium.
A kind of reducing in the production method producing PVB resin displacement above-mentioned, the sulfonate of described emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium weight ratio are (1～2): 1 or 1:(1～2).
In above-mentioned a kind of production method reducing production PVB resin displacement, described PVA: butyraldehyde: hydrochloric acid: the ratio of weight and number of additive=(140～160): (80～100): (20～30): 1.
The advantage that the present invention highlights compared to existing technology is:
After the waste water reclamation of soda, drying drying operation is utilized by the present invention, the water consumption that can make production PVB resin is down to about 38 tons, has both decreased the production cost of PVB resin, reduces again the quantity of wastewater effluent producing PVB resin simultaneously, reduce use cost, there is the effect of environmental protection simultaneously.
Accompanying drawing illustrates:
Fig. 1 is the process flow diagram of the embodiment of the present invention 1.
Fig. 2 is the process flow diagram of the embodiment of the present invention 2.
Detailed description of the invention:
With specific embodiment, the invention will be further described below:
Embodiment 1, referring to Fig. 1:
A kind of production method reducing production PVB resin displacement, comprises the steps:
(1) dissolve: being put in dissolution kettle by PVA and dissolve, PVA is dissolved into the PVA aqueous solution that concentration is 9～11, general concentration is 10%, and concentration allows there is error；
(2) filter: PVA aqueous solution step (1) dissolved and cold pure water plate type heat exchanger carry out heat exchange cooling；
(3) reaction: step (2) is put in reactor through the PVA aqueous solution of cooling, when PVA aqueous solution is heated to 15～20 DEG C by reactor, put into butyraldehyde, hydrochloric acid, PVA aqueous solution and butyraldehyde, hydrochloric acid react in a kettle., reactant was as a child put to calm still by reaction 0.5～1.5, the present embodiment selective response 1 hour；
(4) calm: step (3) reacted reactant to be heated up in calm still, within 1～5 hour, is warming up to 65～75 DEG C；The temperature of heating-up time and intensification is any value in above-mentioned scope, and the present embodiment selects to be warming up to 70 DEG C in 3 hours.
(5) insulation: after the reactant of step (4) is carried out insulation 0.5～1.5 hour in calm still, reactant is put to washing kettle；Temperature retention time can in above-mentioned scope any value.The present embodiment selects insulation 1 hour.
(6) washing: by the reactant of step (5) with recycling water water washing more than 5 times, specifically: first draining is to washing kettle fixed position, then mend and recycle water to graduation mark place in washing kettle, after stirring 15～25 minutes, draining is to sewage disposal, repeating above-mentioned action more than 5 times, the mixing time of the present embodiment selects 20 minutes.Washing kettle fixed position refers to the position at drain pipe place, namely washing kettle periphery drum-shaped and cancellated soldering opening place.
(7) acid is washed: by the reactant deionized water wash more than 2 times of step (6), specifically: first draining is to washing kettle fixed position, then deionized water is mended to graduation mark place in washing kettle, after stirring 15～25 minutes, draining is to sewage disposal, repeating above-mentioned action more than 2 times, the mixing time of the present embodiment selects 20 minutes；
(8) adding in alkali and hydrochloric acid: add alkali liquor in the reactant of step (7) and be neutralized reaction so that it is pH value reaches 11～13, and keeps more than 2 hours, pH value can any value, the present embodiment selection 12 in above-mentioned scope.
(9) soda: the water in the reactant of step (8) is discharged to recovery pond, then deionized water is mended to washing kettle graduation mark place, again discharge to recovery pond after stirring 15～25 minutes, repeat soda action until the water conductivity of reactant is less than 50 in washing kettle；Mixing time can any value, the present embodiment selection stirring 20 minutes in above-mentioned scope.
(10) waste water reclamation: by step (9) soda produce waste water reclaim, waste water is drained in waste water reclamation pond, the waste water of recovery for next time wash acid operation；
(11) drying is dried: be evacuated in drier by the reactant of step (10) and carry out drying operation
(12) waste water reclamation: by step (11) dry dry produce waste water reclaim, waste water is drained in waste water reclamation pond, the waste water of recovery for next time wash acid operation；
(13) finished product: obtain PVB resin powder.
Above-mentioned PVA: butyraldehyde: the ratio of weight and number of hydrochloric acid=(14～16): (8～10): (2～3), each ratio is any value in above-mentioned scope,
The present embodiment selects: PVA: butyraldehyde: the 14:8:2 of hydrochloric acid；
Or PVA: butyraldehyde: the ratio of weight and number=15:9:2.5 of hydrochloric acid；
Or PVA: butyraldehyde: the ratio of weight and number=16:10:3 of hydrochloric acid.
Embodiment 2, referring to Fig. 2:
The present embodiment is substantially the same manner as Example 1, it is distinctive in that: when step (3), being additionally added additive and promote the reaction of PVA and butyraldehyde, described additive is: the sulfonate (FMES) of emulsifying agent fatty acid methyl ester ethoxylate and the mixture of emulsifying agent alkylbenzene ether sulfonic acid sodium (DBS).
Wherein, the sulfonate (FMES) of described emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium (DBS) weight ratio are (1～2): 1 or 1:(1～2), can in above-mentioned scope any value, the present embodiment select 1:1.
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio of additive=(140～160): (80～100): (20～30): 1, it is possible to any value in above-mentioned scope, the present embodiment selects 150:90:25:1.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 3:
The present embodiment is substantially the same manner as Example 1, and it is distinctive in that: described PVA: butyraldehyde: hydrochloric acid: the weight ratio=140:80:20:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 4:
The present embodiment is substantially the same manner as Example 1, and it is distinctive in that: described PVA: butyraldehyde: hydrochloric acid: the weight ratio=160:100:30:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 5:
The present embodiment is substantially the same manner as Example 2, and it is distinctive in that: the sulfonate (FMES) of described emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium (DBS) weight ratio are 1:1.5.
Embodiment 6:
The present embodiment is substantially the same manner as Example 2, and it is distinctive in that: the sulfonate (FMES) of described emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium (DBS) weight ratio are 1:2.
Embodiment 7:
The present embodiment is substantially the same manner as Example 2, and it is distinctive in that: the sulfonate (FMES) of described emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium (DBS) weight ratio are 2:1.
Embodiment 8:
The present embodiment is substantially the same manner as Example 2, and it is distinctive in that: the sulfonate (FMES) of described emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium (DBS) weight ratio are 1.5:1.
Embodiment 9:
The present embodiment is substantially the same manner as Example 5, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=160:100:30:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 10:
The present embodiment is substantially the same manner as Example 5, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=140:80:20:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 11:
The present embodiment is substantially the same manner as Example 6, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=140:80:20:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 12:
The present embodiment is substantially the same manner as Example 6, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=160:100:30:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 13:
The present embodiment is substantially the same manner as Example 7, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=160:100:30:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 14:
The present embodiment is substantially the same manner as Example 7, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=140:80:20:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 15:
The present embodiment is substantially the same manner as Example 8, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=160:100:30:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Embodiment 16:
The present embodiment is substantially the same manner as Example 8, and it is distinctive in that:
Described PVA: butyraldehyde: hydrochloric acid: the weight ratio=140:80:20:1 of additive.When each dispensing, the gross weight of additive is more than 4Kg.
Above-described embodiment is only one of presently preferred embodiments of the present invention, not limits the practical range of the present invention with this, therefore: the equivalence change that all shapes under this invention, structure, principle are done, all should be covered by within protection scope of the present invention.
Claims (5)
1. one kind is reduced the production method producing PVB resin displacement, it is characterised in that: comprise the steps:
(1) dissolve: PVA is put in dissolution kettle and dissolves, PVA is dissolved into the PVA aqueous solution that concentration is 9～11%；
(2) filter: PVA aqueous solution step (1) dissolved and cold pure water plate type heat exchanger carry out heat exchange cooling；
(3) reaction: step (2) is put in reactor through the PVA aqueous solution of cooling, when PVA aqueous solution is heated to 15～20 DEG C by reactor, put into butyraldehyde, hydrochloric acid, PVA aqueous solution and butyraldehyde, hydrochloric acid react in a kettle., are put to calm still by reactant after reacting 0.5～1.5 hour；
(4) calm: step (3) reacted reactant to be heated up in calm still, within 1～5 hour, is warming up to 65～75 DEG C；
(5) insulation: after the reactant of step (4) is carried out insulation 0.5～1.5 hour in calm still, reactant is put to washing kettle；
(6) washing: by the reactant of step (5) with recycling water washing more than 5 times, specifically: first draining is to washing kettle fixed position, then mend and recycle water to graduation mark place in washing kettle, after stirring 15～25 minutes, draining is to sewage disposal, repeats above-mentioned action more than 5 times；
(7) acid is washed: by the reactant deionized water wash 2 times of step (6), specifically: first draining is to washing kettle fixed position, then mending deionized water to graduation mark place in washing kettle, after stirring 15～25 minutes, draining is to sewage disposal, repeats above-mentioned action more than 2 times；
(8) add in alkali and hydrochloric acid: in the reactant of step (7), add alkali liquor be neutralized reaction so that it is pH value reaches 11～13, and keeps more than 2 hours；
(9) soda: the water in the reactant of step (8) is discharged to recovery pond, then deionized water is mended to washing kettle graduation mark place, again in water discharge to recovery pond, soda action will be repeated until the water conductivity of reactant is less than 50 in washing kettle after stirring 15～25 minutes；
(10) waste water reclamation: by step (9) soda produce waste water reclaim, waste water is drained in waste water reclamation pond, the waste water of recovery for next time wash acid operation；
(11) drying is dried: be evacuated in drier by the reactant of step (10) and carry out drying operation；
(12) waste water reclamation: by step (11) dry dry produce waste water reclaim, waste water is drained in waste water reclamation pond, the waste water of recovery for next time wash acid operation；
(13) finished product: obtain PVB resin powder.
2. a kind of production method reducing production PVB resin displacement according to claim 1, it is characterised in that: described resin: butyraldehyde: the weight ratio of hydrochloric acid=(14～16): (8～10): (2～3).
3. a kind of production method reducing production PVB resin displacement according to claim 1, it is characterized in that: being additionally added additive in step (3) and promote the reaction of PVA and butyraldehyde, described additive is: the mixture of the sulfonate of emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium.
4. according to claim 3 a kind of reduce the production method producing PVB resin displacement, it is characterised in that: the sulfonate of described emulsifying agent fatty acid methyl ester ethoxylate and emulsifying agent alkylbenzene ether sulfonic acid sodium weight ratio are (1～2): 1 or 1:(1～2).
5. a kind of production method reducing production PVB resin displacement according to claim 3, it is characterised in that: described PVA: butyraldehyde: hydrochloric acid: the ratio of weight and number of additive=(140～160): (80～100): (20～30): 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585906A (en) * | 2017-09-05 | 2018-01-16 | 宜春市康盛高分子材料科技有限公司 | The processing method of waste water in polyvinyl butyral resin preparation process |
| CN113943385A (en) * | 2021-11-19 | 2022-01-18 | 大冶海通热工技术有限公司 | PVB production process based on plate heat exchanger cooling |
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2016
- 2016-04-23 CN CN201610260926.3A patent/CN105713118B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585906A (en) * | 2017-09-05 | 2018-01-16 | 宜春市康盛高分子材料科技有限公司 | The processing method of waste water in polyvinyl butyral resin preparation process |
| CN113943385A (en) * | 2021-11-19 | 2022-01-18 | 大冶海通热工技术有限公司 | PVB production process based on plate heat exchanger cooling |
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Denomination of invention: A production method to reduce the displacement of PVB resin Effective date of registration: 20200909 Granted publication date: 20180717 Pledgee: Zheshang Bank Limited by Share Ltd. Taizhou branch Pledgor: ZHEJIANG DECENT NEW MATERIAL Co.,Ltd. Registration number: Y2020330000682 |