CN103143340B - Catalyst applied to n-dodecanol ester synthesis and preparation method thereof - Google Patents
Catalyst applied to n-dodecanol ester synthesis and preparation method thereof Download PDFInfo
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- CN103143340B CN103143340B CN201310076363.9A CN201310076363A CN103143340B CN 103143340 B CN103143340 B CN 103143340B CN 201310076363 A CN201310076363 A CN 201310076363A CN 103143340 B CN103143340 B CN 103143340B
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Abstract
The invention discloses a catalyst applied to n-dodecanol ester synthesis. The catalyst is a powder product and comprises the following ingredients by weight percent: 15-22% of sodium hydroxide, 15-26% of calcium hydroxide, 15-25% of barium hydroxide, 15-30% of magnesium hydrate and 17-25% of zinc hydroxide. The invention further discloses a preparation method of the catalyst applied to n-dodecanol ester synthesis. The preparation method comprises the following specific steps of: firstly, measuring the ingredients according to the proportion; secondly, feeding the measured ingredients into a ball mill to be milled for 20-24 hours; and finally screening the ingredients by using a screen of which the aperture is 0.070-0.074mm so as to obtain a finished product. The target product is dissolved into emulsion paint, and the emulsion particles are sufficiently swelled, so that the emulsion paint is good in filming continuity and compact, smooth and uniform paint films are easy to form; the paint films are greatly improved in scrubbing resistance, color revealing capability, glossiness and weather resistance, and what is more important is that isobutyraldehyde which is catalyzed by using the catalyst is high in reaction conversion rate and less in byproduct.
Description
Technical field
The present invention relates to a kind of Catalysts and its preparation method for the synthesis of coalescents, specifically, the present invention relates to a kind of for the synthetic Catalysts and its preparation method of Lauryl Alcohol ester.
Background technology
Lauryl Alcohol ester is a kind of strong solvent of latex base polymer, be widely used among the multiple emulsion such as pure third, phenylpropyl alcohol, vinegar third, silicon third and polyvinyl acetate that comprises high pH value, its hydrolysis property is stable, and coalescent performance is high, easily being absorbed by latex particle, is one of at present best coalescents.Since last century the eighties, the raw material of producing Lauryl Alcohol ester is isobutylaldehyde always, carries out condensation esterification synthetic with NaOH as catalyst.This kind of traditional handicraft is simple, ripe, can industrially produce the Lauryl Alcohol ester supply market of high-quality.But prior art exists as catalyst the problem that reaction conversion ratio is low, accessory substance is many with NaOH, causes production cost high, deficiency in economic performance, directly affects market sales volume.
Summary of the invention
The present invention is mainly for the deficiencies in the prior art, propose a kind of taking multiple alkali as raw material for the preparation of the synthetic catalyst of Lauryl Alcohol ester, this catalytic component is simple, wide material sources, low-consuming, conversion ratio is high, accessory substance is few.The present invention also comprises the method for preparing catalyst synthetic for Lauryl Alcohol ester.
The present invention is achieved through the following technical solutions technical goal.
For the synthetic catalyst of Lauryl Alcohol ester, it is powder, and its improvements are: components based on weight percentage amount is as follows: NaOH 15%～22%, calcium hydroxide 15%～26%, barium hydroxide 15%～25%, magnesium hydroxide 15%～30% and zinc hydroxide 17%～25%.
As further improvement project, the preferential range of choice of the consumption of calcium hydroxide is 18%～22%, and the preferential range of choice of consumption of barium hydroxide is 16%～20%.
As further improvement project, above-mentioned barium hydroxide is barium monohydrate or barium hydroxide.
The present invention also comprises the method for preparing catalyst synthetic for Lauryl Alcohol ester, concrete enforcement by following process steps:
(1) get the raw materials ready by proportioning metering raw material;
(2) ball milling will be put in ball mill through the raw material of metering, ball milling 20～24 hours;
(3) screening is that 0.070～0.074mm screen cloth filters out finished product with aperture.
The present invention compared with prior art, has following good effect:
1, target product of the present invention is soluble in emulsion paint, and latex particle obtains fully swelling, and film forming continuity is good, easily forms tight, level and smooth, uniform paint film, and after this drying varniss, scrub resistance, color developing and glossiness are significantly improved.
2, target product of the present invention mixes that in latex, latex particle to be obtained fully swelling, directly improves paint film wet film performance, significantly improves paint film levelability and hangs fluidity.
3, target product of the present invention mixes in latex, directly improves coalescent between latex particle, significantly reduces the permeability of coating to water vapour, thereby promotes weather resistance.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
The present invention is a kind of for the synthetic catalyst of Lauryl Alcohol ester, it is powder, and components based on weight percentage amount is as follows: NaOH 15%～22%, calcium hydroxide 15%～26%, barium hydroxide 15%～25%, magnesium hydroxide 15%～30% and zinc hydroxide 17%～25%.
The present invention also comprises the method for preparing catalyst synthetic for Lauryl Alcohol ester, and the method is undertaken by following process steps:
(1) get the raw materials ready by proportioning metering raw material;
(2) ball milling will be put in ball mill through the raw material of metering, ball milling 20～24 hours;
(3) screening is that 0.070～0.074mm screen cloth filters out finished product with aperture.
Now further illustrate the technology of the present invention effect by embodiment and application examples, see the following form for the synthetic catalyst Preparation Example of Lauryl Alcohol ester, to be applied to actual production for the synthetic catalyst of Lauryl Alcohol ester, use the Lauryl Alcohol ester weight of making to carry out confirmatory reaction conversion ratio.
For the synthetic catalyst Preparation Example of Lauryl Alcohol ester
Application examples 1
First, take 20 tons of raw material isobutylaldehydes, feedstock pump is delivered in synthesis reactor, in still, ceaselessly stir raw material, 25 kilograms of the catalyst that order is made toward the interior input of the synthesis reactor embodiment of the present invention 1, are heated to 55 DEG C ± 3 DEG C with the speed of 5 DEG C of intensifications per minute, close when the time comes heating valve.Now in still, start synthetic reaction, and occur refluxing, temperature continues to rise, and in the time that temperature rises to 85 DEG C ± 3 DEG C, closing volume valve, collects unreacted isobutylaldehyde, wait to reflux when obviously minimizing, reopen heating valve, continue to reclaim unreacted isobutylaldehyde by intensification, in the time that temperature rises to 120 DEG C ± 3 DEG C, slowly open vacuum valve, receive unreacted isobutylaldehyde to the greatest extent, again close heating valve.Observe no liquid while occurring by backflow visor, then close vacuum valve, wait to be cooled to 45 DEG C ± 3 DEG C and filter dischargings, should use-case obtain 17.58 tons of the Lauryl Alcohol esters of content >=98%.
Application examples 2
First, take 20 tons of raw material isobutylaldehydes, feedstock pump is delivered in synthesis reactor, in still, ceaselessly stir raw material, 25 kilograms of the catalyst that order is made toward the interior input of the synthesis reactor embodiment of the present invention 2, are heated to 55 DEG C ± 3 DEG C with the speed of 5 DEG C of intensifications per minute, close when the time comes heating valve.Now in still, start synthetic reaction, and occur refluxing, temperature continues to rise, and in the time that temperature rises to 85 DEG C ± 3 DEG C, closing volume valve, collects unreacted isobutylaldehyde, wait to reflux when obviously minimizing, reopen heating valve, continue to reclaim unreacted isobutylaldehyde by intensification, in the time that temperature rises to 120 DEG C ± 3 DEG C, slowly open vacuum valve, receive unreacted isobutylaldehyde to the greatest extent, again close heating valve.Observe no liquid while occurring by backflow visor, then close vacuum valve, wait to be cooled to 45 DEG C ± 3 DEG C and filter dischargings, should use-case obtain 17.62 tons of the Lauryl Alcohol esters of content >=98%.
The weight of making the Lauryl Alcohol ester of content >=98% from above-mentioned two application examples, reaction conversion ratio all exceedes 88%, because reaction conversion ratio is high, significantly reduces production costs, and improves the market competitiveness.
Claims (4)
1. one kind for the synthetic catalyst of Lauryl Alcohol ester, it is powder, it is characterized in that: components based on weight percentage amount is as follows: NaOH 15%～22%, calcium hydroxide 15%～26%, barium hydroxide 15%～25%, magnesium hydroxide 15%～30% and zinc hydroxide 17%～25%.
2. according to claim 1 for the synthetic catalyst of Lauryl Alcohol ester, it is characterized in that: the amount ranges of calcium hydroxide is 18%～22%, the amount ranges of barium hydroxide is 16%～20%.
3. according to claim 1 for the synthetic catalyst of Lauryl Alcohol ester, it is characterized in that: barium hydroxide is barium monohydrate or barium hydroxide.
4. the preparation method for the synthetic catalyst of Lauryl Alcohol ester according to claim 1, is characterized in that: undertaken by following process steps:
(1) get the raw materials ready by proportioning metering raw material;
(2) ball milling will be put in ball mill through the raw material of metering, ball milling 20～24 hours;
(3) screening is that 0.070～0.074mm screen cloth filters out finished product with aperture.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310076363.9A CN103143340B (en) | 2013-02-06 | 2013-02-06 | Catalyst applied to n-dodecanol ester synthesis and preparation method thereof |
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| CN201310076363.9A CN103143340B (en) | 2013-02-06 | 2013-02-06 | Catalyst applied to n-dodecanol ester synthesis and preparation method thereof |
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| CN103143340A CN103143340A (en) | 2013-06-12 |
| CN103143340B true CN103143340B (en) | 2014-08-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106362776B (en) * | 2016-08-10 | 2019-06-07 | 福州大学 | For synthesizing the catalyst and its preparation method and application of Lauryl Alcohol ester |
| CN107954871A (en) * | 2017-10-27 | 2018-04-24 | 江门谦信化工发展有限公司 | The preparation method of one kind 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates |
| CN111889131B (en) * | 2020-08-20 | 2023-04-28 | 润泰化学（泰兴）有限公司 | Double-base catalyst for catalytic synthesis of 2,4 trimethyl 1,3 pentanediol isobutyrate isooctanoate and preparation method thereof |
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| DE10207745A1 (en) * | 2001-02-22 | 2002-09-05 | Basf Ag | Production of 2,2,4-trimethyl-1,3-pentanediol mono- and diisobutyrate, useful as additives in manufacture of e.g. adhesives and coloring agents, comprises e.g. treating isobutyraldehyde with aqueous alkalimetalhydroxide as basic catalyst |
| CN1173924C (en) * | 2001-11-09 | 2004-11-03 | 吉化集团吉林市江南研究院有限责任公司 | Prepn of 2,2,4-trimethy1-1,3-pentanediol monoisobutyrate |
| CN1260204C (en) * | 2001-12-30 | 2006-06-21 | 中国石化集团齐鲁石油化工公司 | Preparation process of 2,2,4-trimethyl-1,3-pentanediol mono-sio butyrate |
| CN100361955C (en) * | 2006-03-03 | 2008-01-16 | 华东师范大学 | Production of 2,2,4-trimethyl-1,-3-pentadiol mono-isobutyric acid |
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