CN109293803A - A kind of method of production of low-temperature polyethylene butyral composition - Google Patents
A kind of method of production of low-temperature polyethylene butyral composition Download PDFInfo
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- CN109293803A CN109293803A CN201811193256.3A CN201811193256A CN109293803A CN 109293803 A CN109293803 A CN 109293803A CN 201811193256 A CN201811193256 A CN 201811193256A CN 109293803 A CN109293803 A CN 109293803A
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- polyvinyl alcohol
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The present invention to be provided a kind of method of production of low-temperature polyethylene butyral composition.Hydroxy radical content is 36% or so, and butyl content is between 60-63%, and for viscosity in 15-25mpas, molecular weight is 19000 or so.It can be widely used for paint/coating, the fields such as oil covers, cerarrics adhesive, hot melt adhersive, thermoplastic adhesives.
Description
Technical field
The present invention relates to a kind of methods of production of low-temperature polyethylene butyral composition, belong to high molecular material preparation skill
Art field.
Background technique
Polyvinyl butyral is commonly called as PVB, and product itself is a kind of widely used high molecular material, with good
Flexibility, flexing, transparency and mist degree etc..The polyvinyl butyral of the low acetalizing degree of polyhydroxy can be widely used for paint/coating,
The fields such as oil covers, cerarrics adhesive, hot melt adhersive, thermoplastic adhesives.
The main physical and chemical index of low-temperature polyethylene butyral composition are as follows: 36% or so, butyl content exists hydroxy radical content
Between 60-63%, for viscosity in 15-25mpas, molecular weight is 19000 or so.
Currently, the low-temperature polyethylene butyral composition product blank out that China is domestic, so, domestic market is always
It is occupied by Japanese ponding and Kuraray, it is not only expensive, and also transportation cost is also high, haulage time is long.
Summary of the invention
The technical problem to be solved by the present invention is to need to provide a kind of development of low-temperature polyethylene butyral composition
Method.
A kind of above-mentioned purpose that the invention is realized by the following technical scheme: development of low-temperature polyethylene butyral composition
Method is prepared by each raw material of following mass parts: 4-6 parts of low polymerization degree high alcoholysis degree polyvinyl alcohol, the low alcohol of low polymerization degree
4-6 parts of solution degree polyvinyl alcohol, 90-120 parts of deionized water, 5 parts of butyraldehyde, 3-5 parts of concentrated hydrochloric acid.
Preferably, the mass parts of each raw material are as follows: 5 parts of the high alcoholysis degree polyvinyl alcohol of low polymerization degree, the low alcoholysis of low polymerization degree
5 parts of polyvinyl alcohol, 110 parts of deionized water, 5 parts of butyraldehyde, 3.5 parts of concentrated hydrochloric acid of degree.
Specifically, the degree of polymerization of the high alcoholysis degree polyvinyl alcohol of low polymerization degree is 300, alcoholysis degree 98%, the oligomerization
The degree of polymerization for spending polyvinyl alcohol with low alcoholysis level is 300, alcoholysis degree 80%.
A kind of low-temperature polyethylene butyral composition as stated in claim 1 or 2, comprising the following steps:
(1) polyvinyl alcohol of low polymerization degree low alcoholysis level is added to deionized water, room temperature, is stirred, until being completely dissolved, shape
At homogeneous latex emulsion, then, be added the high alcoholysis degree of low polymerization degree polyvinyl alcohol, heating, until temperature in the kettle 95-100 DEG C it
Between, insulated and stirred 2 hours.
(2) into above-mentioned poly-vinyl alcohol solution, n-butanal is added in 30-35 DEG C, by the way of gradient cooling, to kettle
Interior temperature is reduced to 2-4 DEG C, puts into hydrochloric acid, and kept for 1 hour, until product is precipitated completely.
(3) said mixture material is heated, heating rate is 4 DEG C/h, until temperature in the kettle rises to 22-24 DEG C, is protected
It holds 1 hour.(4) with the originally above-mentioned polyvinyl butyral of water washing until the PH of cleaning solution is 7, the then powder after dry washing
End is to get the low acetalizing degree polyvinyl butyral of polyhydroxy.
The beneficial effects of the present invention are: the present invention uses different alcoholysis degrees, the polyvinyl alcohol of same polymeric degree, with hydrochloric acid
With n-butanal carry out aldolisation, prepare low-temperature polyethylene butyral composition jointly, not only resulting product stable structure,
Hydroxyl is high, acetalizing degree is low, moreover, simple process, easily prepared, is suitble to promote the use of.
Specific embodiment
Invention is further described below with reference to example:
Embodiment 1
(1) polyvinyl alcohol of 4 parts of low polymerization degree low alcoholysis levels is added to 90 parts of deionized waters, room temperature, is stirred, until completely
Dissolution forms homogeneous latex emulsion, then, the polyvinyl alcohol of the high alcoholysis degree of 6 low polymerization degrees, heating is added, until temperature in the kettle is 100
Between DEG C, insulated and stirred 2 hours.
(2) into above-mentioned poly-vinyl alcohol solution, 5 parts of n-butanals are added in 30 DEG C, by the way of gradient cooling, to kettle
Interior temperature is reduced to 2 DEG C, puts into 5 parts of hydrochloric acid, and kept for 1 hour, until product is precipitated completely.
(3) said mixture material is heated, heating rate is 4 DEG C/h, until temperature in the kettle rises to 22 DEG C, keeps 1
Hour.
(4) with the originally above-mentioned polyvinyl butyral of water washing until the PH of cleaning solution is 7, the then powder after dry washing
End is to get low-temperature polyethylene butyral composition.
Embodiment 2
(1) polyvinyl alcohol of 5 parts of low polymerization degree low alcoholysis levels is added to 100 parts of deionized waters, room temperature, is stirred, until complete
Fully dissolved forms homogeneous latex emulsion and the polyvinyl alcohol of 5 parts of high alcoholysis degrees of low polymerization degree then is added, heat up, until temperature in the kettle
Between 95 DEG C, insulated and stirred 2 hours.
(2) into above-mentioned poly-vinyl alcohol solution, 5 parts of n-butanals are added in 33 DEG C, by the way of gradient cooling, to kettle
Interior temperature is reduced to 3 DEG C, puts into 3 parts of hydrochloric acid, and kept for 1 hour, until product is precipitated completely.
(3) said mixture material is heated, heating rate is 4 DEG C/h, until temperature in the kettle rises to 24 DEG C, keeps 1
Hour.
(4) with the originally above-mentioned polyvinyl butyral of water washing until the PH of cleaning solution is 7, the then powder after dry washing
End is to get low-temperature polyethylene butyral composition.
Embodiment 3
(1) polyvinyl alcohol of 5 parts of low polymerization degree low alcoholysis levels is added to 120 parts of deionized waters, room temperature, is stirred, until complete
Fully dissolved forms homogeneous latex emulsion and the polyvinyl alcohol of 5 parts of high alcoholysis degrees of low polymerization degree then is added, heat up, until temperature in the kettle
Between 100 DEG C, insulated and stirred 2 hours.
(2) into above-mentioned poly-vinyl alcohol solution, 5 parts of n-butanals are added in 35 DEG C, by the way of gradient cooling, to kettle
Interior temperature is reduced to 2 DEG C, puts into 4 parts of hydrochloric acid, and kept for 1 hour, until product is precipitated completely.
(3) said mixture material is heated, heating rate is 4 DEG C/h, until temperature in the kettle rises to 24 DEG C, keeps 1
Hour.
(4) with the originally above-mentioned polyvinyl butyral of water washing until the PH of cleaning solution is 7, the then powder after dry washing
End is to get low-temperature polyethylene butyral composition.
The low-temperature polyethylene butyral composition that above three embodiments obtain, mass difference is little, all has knot
Structure is stablized, and product requirement is fully met.
Above-described embodiment is presently preferred embodiments of the present invention, is not a limitation on the technical scheme of the present invention, as long as
Without the technical solution that creative work can be realized on the basis of the above embodiments, it is regarded as falling into the invention patent
Rights protection scope in.
Claims (5)
1. a kind of method of production of low-temperature polyethylene butyral composition, which is characterized in that by each raw material of following mass parts
It is prepared: 4-6 parts of low polymerization degree high alcoholysis degree polyvinyl alcohol, 4-6 parts of low polymerization degree polyvinyl alcohol with low alcoholysis level, deionized water
90-120 parts, 5 parts of butyraldehyde, 3-5 parts of concentrated hydrochloric acid.
2. low-temperature polyethylene butyral composition according to claim 1, which is characterized in that the mass parts of each raw material
Are as follows: 5 parts of the high alcoholysis degree polyvinyl alcohol of low polymerization degree, 5 parts of low polymerization degree polyvinyl alcohol with low alcoholysis level, 110 parts of deionized water, butyraldehyde
5 parts, 3.5 parts of concentrated hydrochloric acid.
3. according to claim 1 or low-temperature polyethylene butyral composition described in 2, it is characterised in that the oligomerization
The degree of polymerization for spending high alcoholysis degree polyvinyl alcohol is 300, alcoholysis degree 98%.
4. the degree of polymerization of low polymerization degree polyvinyl alcohol with low alcoholysis level described in is 300, alcoholysis degree 80%.
5. low-temperature polyethylene butyral composition described in claims 1 or 2, it is characterised in that: the following steps are included:
(1) polyvinyl alcohol of low polymerization degree low alcoholysis level is added to deionized water, room temperature, is stirred, until being completely dissolved, formed equal
Then the polyvinyl alcohol of the high alcoholysis degree of low polymerization degree, heating is added in even lotion, until temperature in the kettle between 95-100 DEG C, is protected
Temperature stirring 2 hours；(2) into above-mentioned poly-vinyl alcohol solution, n-butanal is added in 30-35 DEG C, by the way of gradient cooling,
It is reduced to 2-4 DEG C to temperature in the kettle, puts into hydrochloric acid, and kept for 1 hour, until product is precipitated completely；(3) to said mixture material
It is heated, heating rate is 4 DEG C/h, until temperature in the kettle rises to 22-24 DEG C, is kept for 1 hour；(4) in originally water washing
Polyvinyl butyral is stated until the PH of cleaning solution is 7, then the powder after dry washing is to get low-temperature polyethylene butyral
Composition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811193256.3A CN109293803A (en) | 2018-10-14 | 2018-10-14 | A kind of method of production of low-temperature polyethylene butyral composition |
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| CN201811193256.3A CN109293803A (en) | 2018-10-14 | 2018-10-14 | A kind of method of production of low-temperature polyethylene butyral composition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861315A (en) * | 2021-09-18 | 2021-12-31 | 忠信（清远）光伏材料科技有限公司 | Polyvinyl butyral with sound insulation performance and preparation method thereof |
| CN114874575A (en) * | 2021-12-07 | 2022-08-09 | 广安职业技术学院 | Low-density small-aperture polyvinyl formal foam material |
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|---|---|---|---|---|
| JP2001288215A (en) * | 2000-04-06 | 2001-10-16 | Sekisui Chem Co Ltd | Method for manufacturing polyvinyl acetal resin |
| CN103193905A (en) * | 2013-04-03 | 2013-07-10 | 东莞市龙怡阻燃材料有限公司 | Low-viscosity polyvinyl butyral resin as well as preparation method and application thereof |
| CN107022041A (en) * | 2017-04-28 | 2017-08-08 | 成都玉龙化工有限公司 | A kind of high viscosity polyvinyl butyral resin and preparation method thereof |
| CN108070042A (en) * | 2017-11-02 | 2018-05-25 | 成都玉龙化工有限公司 | A kind of full aqueous polyethylene butyral formula and preparation method thereof |
| CN108440693A (en) * | 2018-04-19 | 2018-08-24 | 怀集县怀德新材料有限公司 | A kind of high fusion index resin and preparation method thereof |
-
2018
- 2018-10-14 CN CN201811193256.3A patent/CN109293803A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001288215A (en) * | 2000-04-06 | 2001-10-16 | Sekisui Chem Co Ltd | Method for manufacturing polyvinyl acetal resin |
| CN103193905A (en) * | 2013-04-03 | 2013-07-10 | 东莞市龙怡阻燃材料有限公司 | Low-viscosity polyvinyl butyral resin as well as preparation method and application thereof |
| CN107022041A (en) * | 2017-04-28 | 2017-08-08 | 成都玉龙化工有限公司 | A kind of high viscosity polyvinyl butyral resin and preparation method thereof |
| CN108070042A (en) * | 2017-11-02 | 2018-05-25 | 成都玉龙化工有限公司 | A kind of full aqueous polyethylene butyral formula and preparation method thereof |
| CN108440693A (en) * | 2018-04-19 | 2018-08-24 | 怀集县怀德新材料有限公司 | A kind of high fusion index resin and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 赵容等: "沉淀法合成聚乙烯醇缩丁醛及其应用性能研究", 《中国胶粘剂》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861315A (en) * | 2021-09-18 | 2021-12-31 | 忠信（清远）光伏材料科技有限公司 | Polyvinyl butyral with sound insulation performance and preparation method thereof |
| CN114874575A (en) * | 2021-12-07 | 2022-08-09 | 广安职业技术学院 | Low-density small-aperture polyvinyl formal foam material |
| CN114874575B (en) * | 2021-12-07 | 2024-01-26 | 广安职业技术学院 | Low-density small-pore-size polyvinyl formal foam material |
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Application publication date: 20190201 |