CN103030835A - Parabens plastifying-viscosity reducer and preparation method thereof - Google Patents
Parabens plastifying-viscosity reducer and preparation method thereof Download PDFInfo
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- CN103030835A CN103030835A CN2012105093501A CN201210509350A CN103030835A CN 103030835 A CN103030835 A CN 103030835A CN 2012105093501 A CN2012105093501 A CN 2012105093501A CN 201210509350 A CN201210509350 A CN 201210509350A CN 103030835 A CN103030835 A CN 103030835A
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Abstract
The invention relates to the production of high polymer materials, especially to a parabens plastifying-viscosity reducer and a preparation method thereof. The parabens plastifying-viscosity reducer comprises the following raw materials in parts by weight: 1.2-2.0 parts of 2-propyl heptanol, and 1 part of benzoic acid or phthalic anhydride coproduct. The invention has the advantages of favorable reduced viscosity effect, low quality loss and the like, and can effectively replace the viscosity reducer commonly used on the market, and meanwhile the viscosity in the invention can easily realize industrial production in large scales.
Description
Technical field
The present invention relates to the manufacturing of additives for plastics, specifically a kind of benzoates plasticising, visbreaking agent and preparation method thereof.
Background technology
Common visbreaking agent in the market, kind is few, and the alternative product of downstream client is less, and most of low-grade visbreaking agent all exists boiling point lower, and the course of processing amount of being fuming is large, and mass loss is also more.The visbreaking agent that is applied in the PVC system commonly used on the market mainly contains 2,2,4-trimethylammonium-1, the two isobutyrates of 3-pentanediol (trade(brand)name: TXIB) and fat hydrocarbon (such as D-80) etc.The former all shows well at aspects such as viscosity reducing capability, smell, volatility, use also comparatively extensive, but because its high price, many producers seek cheaper alternative one after another.Fat hydrocarbon is exactly the low-grade visbreaking agent of a modal class, but its shortcoming is obvious too, volatile loss, and taste is large.
Summary of the invention
Technical problem to be solved by this invention is, provides that a kind of thinning effect is good, mass loss is low, realizes easily benzoates plasticising, visbreaking agent of large-scale commercial production and preparation method thereof.
Benzoates plasticising of the present invention, visbreaking agent are made by the raw material of following parts by weight: 1.2～2.0 parts of 2-propyl enanthols, 1 part of phenylformic acid or by-product of benzoic anhydride.By-product of benzoic anhydride refers to the thing that gently boils that produces in the phthalic anhydride production process, and major ingredient is phenylformic acid (BA), phthalic anhydride (PA) and a little unknown impuritie.
The preparation method of benzoates plasticising of the present invention, visbreaking agent is:
The first step, in the reactor that thermometer, distillation condensing works, reflux, whipping appts are housed, add 1.2～2.0 parts of 2-propyl enanthols and 1 part of phenylformic acid or phthalic anhydride byproduct, stirring is warming up to 90 ℃～95 ℃, and phenylformic acid or by-product of benzoic anhydride are dissolved fully;
Second step is warming up to 160～180 ℃ of beginning water outlets, and to heat up in a steamer a temperature be 85～110 ℃ in control in the reaction process; Continue to be warming up to 225 ℃, carried out esterification 2～5 hours, to acid number less than 1.0mgKOH/g;
The 3rd the step, the beginning dealcoholysis to pure mass content less than 1.0%;
In the 4th step, add alkali lye and be neutralized to acid number less than 0.5mgKOH/g;
The 5th the step, be cooled to after the stirring 100～110 ℃ of decompression dehydrations to moisture mass percent less than 0.05%;
The 6th step added gac, silicon bath soil decolorization filtering, obtained the finished product benzoic ether.
In the reactions steps in described five steps of the first step to the, all or part of step is carried out under nitrogen atmosphere protection.
In the raw material of the present invention, phenylformic acid is that chemical industry common are machine acid, moderate, with itself and unit alcohol direct esterification gained esterification products, be applied in the PVC goods as visbreaking agent, have the advantages such as thinning effect is good, mass loss is low, can effectively replace visbreaking agent common on the market, visbreaking agent of the present invention is realized large-scale commercial production easily simultaneously.Product sexual valence of the present invention is higher, and range of application is also extremely extensive, can be applicable to other emulsifying powder application, rubber or the coating such as medical glove, sealing material, tablecloth.
Embodiment
Preparation Example of the present invention is as follows:
The first step: in the reactor that thermometer, distillation condensing works (chuck is arranged), reflux, whipping appts are housed, add 2.0 parts of 2-propyl enanthols (2-PH) and 1 part of phenylformic acid, stirring is warming up to 95 ℃, kept this temperature 1 hour, phenylformic acid is dissolved fully, second step: be warming up to 160～180 ℃ of beginning water outlets, to heat up in a steamer a temperature be 85～110 ℃ in control in the reaction process; Continue to be warming up to 225 ℃, carried out esterification 4 hours, to acid number less than 0.5mgKOH/g; The 3rd step: the beginning dealcoholysis to pure content less than the 0.1%(mass percent), the 4th step: add alkali lye and be neutralized to acid number less than 0.3mgKOH/g, the 5th step: stir be cooled to behind the 15min 110 ℃ of decompression dehydrations to moisture mass percent less than 0.05%; The 6th step: add gac, silicon bath soil decolorization filtering, obtain the finished product benzoic ether.In the reactions steps in five steps of the first step to the, all or part of step is carried out under nitrogen atmosphere protection, causes the finished color xanthochromia to prevent material and airborne oxygen generation side reaction.
The product performance of the embodiment of the invention detect as follows:
1. product voltinism detected result:
2. the processed and applied Performance Ratio
2.1.25 ℃ PHB and TXIB mould stick with paste through the time stability of viscidity relatively
Test formulations PRG (100) DINP (80) CZF990 (2.4) PHB/TXIB (20)
From upper table data can find out product P HB of the present invention mould stick with paste through the time outperform TXIB aspect the stability of viscidity.
2.2.PHB take out sheet plasticizing process mass loss data with TXIB
Prescription: PVC--100g, DINP--40g, PHB/TXIB--15g, stablizer--2.4g;
Take out the sheet temperature: 175 ℃, take out sheet time: 5min;
Product P HB of the present invention only is half of TXIB taking out sheet procedure quality loss.
2.3. plasticizing efficiency aspect performance
Prescription: PVC--100g, PHB/TXIB--60g, stablizer--2.4g
The obtained PVC goods of product P HB of the present invention hardness is starkly lower than like product, can judge that plasticizing efficiency is higher than similar visbreaking agent product TXIB.
Claims (3)
1. a benzoates plasticising, visbreaking agent, it is characterized in that: the raw material by following parts by weight is made, 1.2～2.0 parts of 2-propyl enanthols, 1 part of phenylformic acid or by-product of benzoic anhydride.
2. the preparation method of a benzoates plasticising, visbreaking agent is characterized in that:
The first step, in the reactor that thermometer, distillation condensing works, reflux, whipping appts are housed, add 1.2～2.0 parts of 2-propyl enanthols and 1 part of phenylformic acid or by-product of benzoic anhydride, stirring is warming up to 90 ℃～95 ℃, and phenylformic acid or by-product of benzoic anhydride are dissolved fully;
Second step is warming up to 160～180 ℃ of beginning water outlets, and to heat up in a steamer a temperature be 85～110 ℃ in control in the reaction process; Continue to be warming up to 225 ℃, carried out esterification 2～5 hours, to acid number less than 1.0mgKOH/g;
The 3rd the step, the beginning dealcoholysis to pure mass content less than 1.0%;
In the 4th step, add alkali lye and be neutralized to acid number less than 0.5mgKOH/g;
The 5th the step, be cooled to after the stirring 100～110 ℃ of decompression dehydrations to moisture mass percent less than 0.05%;
The 6th step added gac, silicon bath soil decolorization filtering, obtained the finished product benzoic ether.
3. the preparation method of benzoates plasticising according to claim 2, visbreaking agent is characterized in that: in the reactions steps in described five steps of the first step to the, all or part of step is carried out under nitrogen atmosphere protection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105093501A CN103030835A (en) | 2012-12-03 | 2012-12-03 | Parabens plastifying-viscosity reducer and preparation method thereof |
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| CN2012105093501A CN103030835A (en) | 2012-12-03 | 2012-12-03 | Parabens plastifying-viscosity reducer and preparation method thereof |
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| CN103030835A true CN103030835A (en) | 2013-04-10 |
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| CN2012105093501A Pending CN103030835A (en) | 2012-12-03 | 2012-12-03 | Parabens plastifying-viscosity reducer and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040138358A1 (en) * | 2002-10-26 | 2004-07-15 | Jurgen Koch | Isodecyl benzoate mixtures, preparation, and their use |
| CN101107306A (en) * | 2005-01-18 | 2008-01-16 | 埃克森美孚化学专利公司 | Improvements in or relating to plasticiser compositions |
| CN102741373A (en) * | 2009-11-05 | 2012-10-17 | 巴斯夫欧洲公司 | Adhesives and sealants comprising ester based on 2-propylheptanol |
-
2012
- 2012-12-03 CN CN2012105093501A patent/CN103030835A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040138358A1 (en) * | 2002-10-26 | 2004-07-15 | Jurgen Koch | Isodecyl benzoate mixtures, preparation, and their use |
| CN101107306A (en) * | 2005-01-18 | 2008-01-16 | 埃克森美孚化学专利公司 | Improvements in or relating to plasticiser compositions |
| CN102741373A (en) * | 2009-11-05 | 2012-10-17 | 巴斯夫欧洲公司 | Adhesives and sealants comprising ester based on 2-propylheptanol |
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Application publication date: 20130410 |