CN105713118B - A kind of production method reducing production PVB resin displacement - Google Patents
A kind of production method reducing production PVB resin displacement Download PDFInfo
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- CN105713118B CN105713118B CN201610260926.3A CN201610260926A CN105713118B CN 105713118 B CN105713118 B CN 105713118B CN 201610260926 A CN201610260926 A CN 201610260926A CN 105713118 B CN105713118 B CN 105713118B
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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 present invention relates to a kind of production methods reducing production PVB resin displacement, include the following steps：(1) it dissolves, (2) filtering, (3) reaction, (4) it calms, (5) it keeps the temperature, (6) washing, (7) wash acid, (8) add alkali neutralization hydrochloric acid, (9) soda, (10) Sewage treatment, (11) drying drying, (12) Sewage treatment, (13) finished product；After the present invention utilizes the Sewage treatment of soda, drying drying process, the water consumption of production PVB resin can be made to be down to 38 tons or so, not only reduced the production cost of PVB resin, but also reduce the quantity of wastewater effluent of production PVB resin, use cost is reduced, while having the effect of environmental protection.
Description
Technical field：
The present invention relates to a kind of production methods reducing production PVB resin displacement.
Background technology：
Polyvinyl butyral resin Project Product belongs to thermoplastic macromolecule material field, is polyvinyl butyral
(PVB) main production raw material of glued membrane.PVB resin powder is plasticized through specialty plasticiser, is then squeezed by double screw extruder
It is shaped to PVB glued membranes.PVB glued membranes with its excellent optical property, high temperature resistant, low temperature, mechanical performance and to unorganic glass it is good
Adhesive property become the necessary raw material for producing all kinds of safety glasses.When by extraneous intense impact, PVB glued membranes can be inhaled
Receive impact energy, do not generate flinders, while with security feature, also excellent sound insulation, it is light-operated, heat preservation, it is heat-insulated, anti-
The performances such as mist are ideal safety glass rapidoprints.
The production of external PVB is concentrated mainly on the U.S., Japan and West Europe, estimation total productive capacity oneself reach 130,000 tons with
On.The U.S. is PVB productions and consumes maximum country, and main manufacturer You Shou promises company be (SOLUTION, MANSANTO group
Branch company), E.I.Du Pont Company and union carbide corporation.Shou Nuo companies are maximum PVB manufacturers in the world, account for about whole world PVB productions
The 50% of ability, the product of the said firm are not only used to produce diaphragm, but also for the industries such as priming paint, coating, electrical.The production of E.I.Du Pont Company
Product almost all is that high viscosity PVB resin is used to produce diaphragm, is divided equally with the SEKISUI (ponding company) of Shou Nuo companies, Japan
World PVB films market, there are oneself independent raw material processing enterprise in three companies, for the required resin of pvb film, increasing
Modeling agent and processing technology take stringent secrecy provision.
The development of China PVB be since 1956, by Shenyang Chemical Engineering Inst and Tianjin synthetic material research institute into
The lab scale development work of vinyl acetate and its acetal product is gone.The first designing institute of the Ministry of Chemical Industry in 1958 is Jinxi Chemical Research Institute
Devise the earliest tentative acetal workshop in China.Jinxi Chemical Research Institute in 1961 transfers acetal workshop to Jinxi chemistry work
Organic factory of industry company, the chemical plant of Jinxi in 1964 workshops PVB start to produce as a trial.After the seventies, due to PVB in ceramic marble paper and
The application of aluminium-foil paper industry achieves breakthrough, to promote the development of PVB industries.1985-1988, former China National Light Industrial Products Department takes the lead,
Organize Jinxi chemical plant, Tianjin icy mountain peak chemical plant, Guizhou organic chemical industry's pilot plant, Shanghai optical research institute etc. the country it is strong
Producer has held PVB film decisive battles, it is desirable to be able to realize that safety glass is domesticized with PVB films early, but because of various reasons
Do not succeed, only Guizhou organic chemical industry pilot plant, Shanghai optical research are produced, but yield is relatively low, and quality can not be with import
Product competition.
The high-end PVB of China is all by import, and main cause is production technology and mating insufficient raw material, since PVB is produced
Technique be PVA (polyvinyl alcohol) aqueous solution under the effect of the catalyst with polyvinyl butyral resin, after washing drying become
PVB powder end resin.Compared to external production technology, our equipment and technology seriously falls behind external colleague.And China uses
Be traditional old technology, manufacturing enterprise does not have mating PVB films research institution, this is also to cause high terminal membrane PVB complete
Portion relies on the reason of import.
Traditional PVB production technology water consumption is too high, and ton consumes 100 tons or so, and not only not environmentally, and production cost is also high.
Invention content：
The object of the present invention is to provide a kind of economic, environmental protection additive and utilize its reduction production PVB resin displacement
Production method.
The invention is realized in this way：
A kind of production method reducing production PVB resin displacement, includes the following steps：
(1) it dissolves：Will PVA put into dissolution kettle in dissolve, PVA is dissolved into a concentration of 9~11% PVA it is water-soluble
Liquid；
(2) cool down：The PVA aqueous solutions of step (1) dissolving are subjected to heat exchange cooling with cold pure water with plate heat exchanger；
(3) it reacts：PVA aqueous solution of the step (2) through cooling is put into reaction kettle, when reaction kettle adds PVA aqueous solutions
When heat is to 15~20 DEG C, input butyraldehyde, hydrochloric acid, PVA aqueous solutions are reacted in a kettle with butyraldehyde, hydrochloric acid, and reaction 0.5~
Reactant is put to calm kettle after 1.5 hours；
(4) it calms：Reactant after step (3) is reacted heats up in calm kettle, it is warming up within 1~5 hour 65~
75℃；
(5) it keeps the temperature：After the reactant of step (4) is carried out heat preservation 0.5~1.5 hour in calm kettle, reactant is put
To washing kettle；
(6) it washes：By the reactant of step (5) with water washing 5 times or more is recycled, specifically：First draining is extremely washed
Then kettle fixed position is mended and is recycled in water to washing kettle at graduation mark, stirring drains after 15~25 minutes to sewage disposal,
Repeat above-mentioned action 5 times or more；
(7) acid is washed：The reactant of step (6) is washed with deionized 2 times or more, specifically：It first drains to washing kettle
Then fixed position is mended in deionized water to washing kettle at graduation mark, stirring drains after 15~25 minutes to sewage disposal, repeats
Above-mentioned action 2 times or more；
(8) add alkali neutralization hydrochloric acid：Lye is added in the reactant of step (7) and carries out neutralization reaction, its pH value is made to reach
11~13, and kept for 2 hours or more；
(9) soda：Water in the reactant of step (8) is emitted into recovery pond, then mends deionized water to washing kettle
At graduation mark, water is emitted into recovery pond by stirring again after 15~25 minutes, repeats soda action until reaction in washing kettle
The water conductivity of object is 50 or less；
(10) Sewage treatment：The waste water that step (9) soda generates is recycled, waste water is drained into Sewage treatment pond,
The waste water of recycling for next time wash sour process；
(11) drying drying：The reactant of step (10) is evacuated in dryer and carries out drying operation；
(12) Sewage treatment：Step (11) is dried the waste water that drying generates to recycle, waste water is drained into Sewage treatment
Chi Zhong, the waste water of recycling for next time wash sour process；
(13) finished product：Obtain PVB resin powder.
In the production method that a kind of above-mentioned reduction produces PVB resin displacement, the PVA resins：Butyraldehyde：Hydrochloric acid
Weight ratio=(14~16):(8~10):(2~3).
In the production method that a kind of above-mentioned reduction produces PVB resin displacement, additive is additionally added in step (3)
Promotion PVA is reacted with butyraldehyde, and the additive is：The sulfonate of emulsifier fatty acid methyl ester ethoxylate and emulsifier alkane
The mixture of base phenylate sodium sulfonate.
In the production method that a kind of above-mentioned reduction produces PVB resin displacement, the emulsifier fatty acid methyl ester second
The sulfonate of oxygroup compound is (1~2) with emulsifier alkylbenzene ether sulfonic acid sodium weight ratio:1 or 1：(1~2).
In the production method that a kind of above-mentioned reduction produces PVB resin displacement, the PVA：Butyraldehyde：Hydrochloric acid：Addition
The weight part ratio of agent=(140~160):(80~100):(20~30):1.
The advantage that the present invention protrudes compared with prior art is：
After the present invention utilizes the Sewage treatment of soda, drying drying process, the water consumption of production PVB resin can be made to be down to
38 tons or so, the production cost of PVB resin was not only reduced, but also has reduced the quantity of wastewater effluent of production PVB resin, had reduced
Use cost, while having the effect of environmental protection.
Description of the drawings：
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.
Specific implementation mode：
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, includes the following steps：
(1) it dissolves：PVA is put into dissolution kettle and is dissolved, PVA is dissolved into a concentration of 9~11 PVA aqueous solutions,
For general concentration 10%, concentration allows that there are errors；
(2) cool down：The PVA aqueous solutions of step (1) dissolving are subjected to heat exchange cooling with cold pure water with plate heat exchanger；
(3) it reacts：PVA aqueous solution of the step (2) through cooling is put into reaction kettle, when reaction kettle adds PVA aqueous solutions
When heat is to 15~20 DEG C, input butyraldehyde, hydrochloric acid, PVA aqueous solutions are reacted in a kettle with butyraldehyde, hydrochloric acid, and reaction 0.5~
1.5 as a child put reactant to calm kettle, the present embodiment selection reaction 1 hour；
(4) it calms：Reactant after step (3) is reacted heats up in calm kettle, it is warming up within 1~5 hour 65~
75℃；Arbitrary value, the present embodiment select 3 hours to be warming up to 70 DEG C to the temperature of heating-up time and heating within the above range.
(5) it keeps the temperature：After the reactant of step (4) is carried out heat preservation 0.5~1.5 hour in calm kettle, reactant is put
To washing kettle；Soaking time can arbitrary value within the above range.The present embodiment selection heat preservation 1 hour.
(6) it washes：By the reactant of step (5) with water water washing 5 times or more is recycled, specifically：It first drains to water
Kettle fixed position is washed, then mends and recycles in water to washing kettle at graduation mark, after stirring 15~25 minutes at draining to sewage
Reason repeats above-mentioned action 5 times or more, and the mixing time of the present embodiment selects 20 minutes.Washing kettle fixed position refers to drainpipe
At the position at place, that is, the soldering opening of washing kettle periphery drum-shaped and reticular structure.
(7) acid is washed：The reactant of step (6) is washed with deionized 2 times or more, specifically：It first drains to washing kettle
Then fixed position is mended in deionized water to washing kettle at graduation mark, stirring drains after 15~25 minutes to sewage disposal, repeats
The mixing time of above-mentioned action 2 times or more, the present embodiment selects 20 minutes；
(8) add alkali neutralization hydrochloric acid：Lye is added in the reactant of step (7) and carries out neutralization reaction, its pH value is made to reach
11~13, and kept for 2 hours or more, pH value arbitrary value, the present embodiment can select 12 within the above range.
(9) soda：Water in the reactant of step (8) is emitted into recovery pond, then mends deionized water to washing kettle
At graduation mark, stirring is emitted into recovery pond again after 15~25 minutes, repeats soda action up to reactant in washing kettle
Water conductivity is 50 or less；Mixing time can stir 20 minutes in arbitrary value, the present embodiment selection within the above range.
(10) Sewage treatment：The waste water that step (9) soda generates is recycled, waste water is drained into Sewage treatment pond,
The waste water of recycling for next time wash sour process；
(11) drying drying：The reactant of step (10) is evacuated in dryer and carries out drying operation
(12) Sewage treatment：Step (11) is dried the waste water that drying generates to recycle, waste water is drained into Sewage treatment
Chi Zhong, the waste water of recycling for next time wash sour process；
(13) finished product：Obtain PVB resin powder.
Above-mentioned PVA：Butyraldehyde：The weight part ratio of hydrochloric acid=(14~16):(8~10):(2~3), each ratio is in above-mentioned model
Interior arbitrary value is enclosed,
The present embodiment selects：PVA：Butyraldehyde：The 14 of hydrochloric acid:8:2；
Or PVA：Butyraldehyde：Weight part ratio=15 of hydrochloric acid:9:2.5；
Or PVA：Butyraldehyde：Weight part ratio=16 of hydrochloric acid:10:3.
Embodiment 2, referring to Fig. 2：
The present embodiment is substantially the same manner as Example 1, difference lies in：At step (3), it is additionally added additive and promotes PVA
With reacting for butyraldehyde, the additive is：The sulfonate (FMES) of emulsifier fatty acid methyl ester ethoxylate and emulsifier alkane
The mixture of base phenylate sodium sulfonate (DBS).
Wherein, the sulfonate (FMES) of the emulsifier fatty acid methyl ester ethoxylate and emulsifier alkylbenzene ether sulfonic acid
Sodium (DBS) weight ratio is (1~2):1 or 1：(1~2) arbitrary value, the present embodiment can select 1 within the above range:1.
The PVA：Butyraldehyde：Hydrochloric acid：The weight ratio of additive=(140~160):(80~100):(20~30):1, it can
With arbitrary value within the above range, the present embodiment selection 150:90:25:1.In each dispensing, the total weight of additive is big
In 4Kg.
Embodiment 3：
The present embodiment is substantially the same manner as Example 1, difference lies in：The PVA：Butyraldehyde：Hydrochloric acid：The weight ratio of additive
=140:80:20:1.In each dispensing, the total weight of additive is more than 4Kg.
Embodiment 4：
The present embodiment is substantially the same manner as Example 1, difference lies in：The PVA：Butyraldehyde：Hydrochloric acid：The weight ratio of additive
=160:100:30:1.In each dispensing, the total weight of additive is more than 4Kg.
Embodiment 5：
The present embodiment is substantially the same manner as Example 2, difference lies in：The emulsifier fatty acid methyl ester ethoxylate
Sulfonate (FMES) is 1 with emulsifier alkylbenzene ether sulfonic acid sodium (DBS) weight ratio:1.5.
Embodiment 6：
The present embodiment is substantially the same manner as Example 2, difference lies in：The emulsifier fatty acid methyl ester ethoxylate
Sulfonate (FMES) is 1 with emulsifier alkylbenzene ether sulfonic acid sodium (DBS) weight ratio:2.
Embodiment 7：
The present embodiment is substantially the same manner as Example 2, difference lies in：The emulsifier fatty acid methyl ester ethoxylate
Sulfonate (FMES) is 2 with emulsifier alkylbenzene ether sulfonic acid sodium (DBS) weight ratio:1.
Embodiment 8：
The present embodiment is substantially the same manner as Example 2, difference lies in：The emulsifier fatty acid methyl ester ethoxylate
Sulfonate (FMES) is 1.5 with emulsifier alkylbenzene ether sulfonic acid sodium (DBS) weight ratio:1.
Embodiment 9：
The present embodiment is substantially the same manner as Example 5, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=160 of additive:100:30:1.In each dispensing, additive
Total weight is more than 4Kg.
Embodiment 10：
The present embodiment is substantially the same manner as Example 5, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=140 of additive:80:20:1.In each dispensing, additive it is total
Weight is more than 4Kg.
Embodiment 11:
The present embodiment is substantially the same manner as Example 6, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=140 of additive:80:20:1.In each dispensing, additive it is total
Weight is more than 4Kg.
Embodiment 12：
The present embodiment is substantially the same manner as Example 6, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=160 of additive:100:30:1.In each dispensing, additive
Total weight is more than 4Kg.
Embodiment 13：
The present embodiment is substantially the same manner as Example 7, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=160 of additive:100:30:1.In each dispensing, additive
Total weight is more than 4Kg.
Embodiment 14：
The present embodiment is substantially the same manner as Example 7, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=140 of additive:80:20:1.In each dispensing, additive it is total
Weight is more than 4Kg.
Embodiment 15：
The present embodiment is substantially the same manner as Example 8, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=160 of additive:100:30:1.In each dispensing, additive
Total weight is more than 4Kg.
Embodiment 16：
The present embodiment is substantially the same manner as Example 8, difference lies in：
The PVA：Butyraldehyde：Hydrochloric acid：Weight ratio=140 of additive:80:20:1.In each dispensing, additive it is total
Weight is more than 4Kg.
Above-described embodiment is only one of presently preferred embodiments of the present invention, and but not intended to limit the scope of the present invention, therefore：
The equivalence changes that all shape, structures under this invention, principle are done, should all be covered by within protection scope of the present invention.
Claims (2)
1. a kind of production method reducing production PVB resin displacement, it is characterised in that：Include the following steps：
(1) it dissolves：PVA is put into dissolution kettle and is dissolved, PVA is dissolved into a concentration of 9~11% PVA aqueous solutions；
(2) cool down：The PVA aqueous solutions of step (1) dissolving are subjected to heat exchange cooling with cold pure water with plate heat exchanger；
(3) it reacts：PVA aqueous solution of the step (2) through cooling is put into reaction kettle, when PVA aqueous solutions are heated to by reaction kettle
At 15~20 DEG C, input butyraldehyde, hydrochloric acid, PVA aqueous solutions are reacted in a kettle with butyraldehyde, hydrochloric acid, reaction 0.5~1.5
Reactant is put to calm kettle after hour；The PVA resins：Butyraldehyde：The weight ratio of hydrochloric acid=(14~16):(8~10):(2
~3)；
(4) it calms：Reactant after step (3) is reacted heats up in calm kettle, is warming up to 65~75 DEG C within 1~5 hour；
(5) it keeps the temperature：After the reactant of step (4) is carried out heat preservation 0.5~1.5 hour in calm kettle, reactant is put to water
Wash kettle；
(6) it washes：By the reactant of step (5) with water washing 5 times or more is recycled, specifically：It first drains solid to washing kettle
Positioning is set, and is then mended and is recycled in water to washing kettle at graduation mark, and stirring drains after 15~25 minutes to sewage disposal, repeats
Above-mentioned action 5 times or more；
(7) acid is washed：The reactant of step (6) is washed with deionized 2 times, specifically：It first drains to washing kettle fixed position,
Then it mends in deionized water to washing kettle at graduation mark, stirring drains after 15~25 minutes to sewage disposal, repeats above-mentioned action 2
More than secondary；
(8) add alkali neutralization hydrochloric acid：Lye is added in the reactant of step (7) and carries out neutralization reaction, make its pH value reach 11~
13, and kept for 2 hours or more；
(9) soda：Water in the reactant of step (8) is emitted into recovery pond, then mends deionized water to washing kettle scale
At line, water is emitted into recovery pond by stirring again after 15~25 minutes, repeats soda action up to reactant in washing kettle
Water conductivity is 50 or less；
(10) Sewage treatment：The waste water that step (9) soda generates is recycled, waste water is drained into Sewage treatment pond, is recycled
Waste water for next time wash sour process；
(11) drying drying：The reactant of step (10) is evacuated in dryer and carries out drying operation；
(12) Sewage treatment：Step (11) is dried the waste water that drying generates to recycle, waste water is drained into Sewage treatment pond,
The waste water of recycling for next time wash sour process；
(13) finished product：Obtain PVB resin powder；
It is additionally added additive in step (3) and promotes reacting for PVA and butyraldehyde, the additive is：Emulsifier fatty acid methyl ester
The mixture of the sulfonate and emulsifier alkylbenzene ether sulfonic acid sodium of ethoxylate；
The PVA：Butyraldehyde：Hydrochloric acid：The weight part ratio of additive=(140~160):(80~100):(20~30):1.
2. a kind of production method reducing production PVB resin displacement according to claim 1, it is characterised in that：It is described
The sulfonate of emulsifier fatty acid methyl ester ethoxylate is (1~2) with emulsifier alkylbenzene ether sulfonic acid sodium weight ratio:1 or 1：
(1~2).
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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 |
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