Continuous production method for 2,2,4-trimethyl-1,3-pentanediol isobutyrate

A technology of pentanediol monoisobutyrate and production method, which is applied in the field of continuous preparation of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, and can solve the problem of reaction temperature Low, low selectivity, complicated process, etc., to achieve the effect of simple reaction operation, high product selectivity, and high product purity

Active Publication Date: 2014-10-01
德纳化工滨海有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent CN1098712A discloses a synthetic method using NaOH as a two-step batch process of the catalyzer. The so-called two-step method is that the first step is under the action of dilute lye, and isobutyraldehyde is subjected to low-temperature aldol condensation reaction. The first step is to carry out intramolecular Cannizzaro reaction under the action of concentrated lye, the conversion rate of isobutyraldehyde can reach 69%, and the product selectivity can reach 89%, but there are many disadvantages in this method: low conversion rate, a large amount of By-products, products are difficult to separate, and the process is complex, requiring washing process, large waste water discharge
[0005] Chinese patent CN1429809A discloses a synthesis method using concentrated NaOH solution as a catalyst in a two-stage tubular reaction process. The first-stage tubular reaction temperature is low at 30-40°C; the second-stage tubular reaction temperature is relatively high at about 90°C. ℃, this method can realize liquid-liquid heterogeneous continuous reaction, but the single-pass conversion rate is very low, only 60%, the selectivity is not high, about 88%, and the post-trea

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  • Continuous production method for 2,2,4-trimethyl-1,3-pentanediol isobutyrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Solid base catalyst Cs-K / SiO 2 preparation of

[0030] 1. Preparation of solid base catalyst carrier

[0031] Step (1) Adhesive molding: Grind and sieve commercially available coarse-porous type II microporous silica gel (produced in Qingdao) that has not been roasted to obtain 200-300 mesh silica gel powder as the raw material for rolling balls. The above-mentioned silica gel powder is placed on the stainless steel turntable of the turntable granulator, and the turntable rotates at a speed of 36 rpm. Spray JA-25 silica sol with a concentration of 25% (calculated as SiO2) (the average particle size of the colloidal particles is 10-20nm) on the powder through a spray gun to make rolling ball seeds. Use 0.5-0.7 liters of silica sol per kilogram of silica gel powder. Then slowly add raw material powder and JA-25 silica sol. When the average diameter of the rolled balls (take the average value of 20 grains) reaches 2-3mm, stop adding silica sol, but continue to...

Embodiment 2

[0050] Adopt described two-step method fixed-bed continuous reaction technique to prepare 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, technological process is as follows figure 1 shown, but the removed unreacted isobutyraldehyde is not recycled. Using two series tubular fixed bed reactors, the solid base catalyst Cs-K / SiO in each reactor 2 The total filling volume is 20 liters.

[0051] The first step reaction process is: the raw material of isobutyraldehyde passes through the delivery pump 1 sent to heat exchanger 2 Preheat, then at a space velocity of 0.3 h -1 From the first tubular fixed bed reactor 3 The top enters the catalyst bed for aldol condensation reaction. The reactor inlet temperature was 35°C. Due to the relatively large heat release of the reaction, cooling water was introduced into the shell side to obtain heat, and the reactor outlet temperature was 50°C.

[0052] The second step reaction process is: from the first tubular fixed bed reactor ...

Embodiment 3

[0058] Except that unreacted isobutyraldehyde reclaims and recycles, other conditions are identical with embodiment 2, and the technological process of present embodiment is as follows figure 1 shown.

[0059] The first step reaction process: dealdehyde tower 8 The removed unreacted isobutyraldehyde is returned to the heat exchanger 2 before, and with the transfer pump 1 The conveyed fresh isobutyraldehyde raw material is mixed and enters the heat exchanger 2 warm up. The preheated material is at a space velocity of 0.3h -1 From the first tubular fixed bed reactor 3 The top enters the catalyst bed for aldol condensation reaction. The reactor inlet temperature was 35°C. Due to the intense heat release of the reaction, cooling water was introduced into the shell side of the reactor, and the outlet temperature of the reactor was controlled at 50°C.

[0060] The second step reaction process: from the first tubular fixed bed reactor 3 The aldol condensate disch...

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Abstract

The invention discloses a continuous production method for 2,2,4-trimethyl-1,3-pentanediol isobutyrate. A two-step method fixed bed continuous reaction process and a solid catalyst are adopted, wherein the catalyst is a solid catalyst Cs-K/SiO2 which is prepared by taking spherical silicon oxide as a carrier to carry caesium-potassium double-alkali metal active components. The method comprises the following steps: adopting two serial tubular type fixed bed reactors, firstly feeding a preheated isobutyraldehyde raw material into a first tubular type fixed bed reactor for an aldol condensation reaction, subsequently feeding an obtained an aldol condensation product into a second tubular type fixed bed reactor for intramolecular Cannizzaro reaction, and continuously reacting so as to obtain a target product. Due to adoption of a two-step method fixed bed continuous reaction process, the method is not only high in isobutyraldehyde conversion rate and product selectivity, but also high in production efficiency, simple in reaction operation, beneficial for energy conservation and discharge reduction and has a large-scale continuous industrial production prospect.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and relates to a continuous preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate (abbreviated as alcohol ester-12) is a high-boiling, polyfunctional glycol ester, which is colorless at room temperature Transparent liquid with a boiling point of 255°C, insoluble in water, can be directly or indirectly used as coating additives, lubricants, solvents, plastic additives, etc., and has a wide range of uses. With the increasingly stringent environmental protection regulations and the continuous improvement of water-based architectural coating industry standards, alcohol ester-12 has become a world-renowned water-based architectural coating (usually latex) because of its excellent film-forming effect, non-toxic and harmless, etc. paint), widely used in vinyl acetate homopolymerization and copolymerizatio...

Claims

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Application Information

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IPC IPC(8): C07C67/44C07C69/28B01J23/04
CPCB01J23/002B01J23/04B01J2523/00C07C45/72C07C67/44B01J2523/13B01J2523/15B01J2523/41C07C69/28C07C47/19
Inventor 秦怡生秦旭东杨建国朱红伟陈荣福王伟哈健张学军段启伟
Owner 德纳化工滨海有限公司
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