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Preparation method of 1,3-glycerol diacrylate

A technology of glycerol diacrylate and glycerol, which is applied in the field of preparation of 1,3-propanetriol diacrylate, can solve the problems of purity, technical process needs to be improved, poor decolorization effect, etc., and achieve the judgment of the reaction end point Simple, low volatility, short reaction cycle effect

Active Publication Date: 2016-12-07
ANQING FEIKAI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In the production process of traditional 1,3-propanetriol diacrylate, after the reaction is completed, a reducing agent is directly added for decolorization, which has the disadvantage of poor decolorization effect
In addition, the purity and technological process of its products also need to be improved

Method used

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  • Preparation method of 1,3-glycerol diacrylate
  • Preparation method of 1,3-glycerol diacrylate
  • Preparation method of 1,3-glycerol diacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) 92.09g of glycerol, 151.3g of acrylic acid, 121.7g of cyclohexane, 3.65g of toluenesulfonic acid, 0.243g of p-hydroxyanisole, 0.243g of tetrakis [β-(3,5-di-tert-butyl -4-hydroxyphenyl) propionic acid] pentaerythritol ester mixed, the control reaction temperature is 85 ℃, through air; when the acid value of the system is 15.4mgKOH / g, the esterification reaction ends;

[0047] (2) Cool down to 60°C and keep warm for 1h;

[0048] (3) The reaction system is lowered in temperature and cooled to 30° C., adding a sodium hydroxide solution with a concentration of 5% in excess of 10% of the acid value measured in the organic phase, and a sodium chloride solution with a concentration of 10% for neutralization, washing 2 times, and standing to take upper organic phase;

[0049] (4) After adding 10% hydrochloric acid aqueous solution and 10% sodium chloride solution for pickling and washing for 2 times, take the upper organic phase;

[0050] (5) adding an aqueous solution wit...

Embodiment 2

[0055] (1) 92.09g of glycerol, 158.5g of acrylic acid, 150.4g of n-hexane, 5.01g of methanesulfonic acid, 0.501g of o-methylhydroquinone, 0.501g of bis(2,4-di-tert-butylphenol ) mixed with pentaerythritol diphosphite, and the controlled reaction temperature was 86°C; when the acid value of the system was 28mgKOH / g, the esterification reaction ended;

[0056] (2) Cool down to 65°C and keep warm for 1h;

[0057] (3) The reaction system is cooled to 35° C., and the acid value measured by the organic phase is added with an excess of 10% concentration of 6% sodium hydroxide solution and 15% sodium chloride solution for neutralization, washing 2 times, and standing to take upper organic phase;

[0058] (4) After adding a concentration of 11% aqueous hydrochloric acid solution and a concentration of 15% sodium chloride solution for pickling and washing for 2 times, take the upper organic phase;

[0059] (5) adding 5% aqueous solution of sodium thiosulfate to the upper organic phase...

Embodiment 3

[0064] (1) 92.09g of glycerol, 165.7g of acrylic acid, 180.5g of toluene, 7.73g of solid superacid, 0.77g of phenothiazine, 0.77g of 2,6-di-tert-butyl-p-cresol are mixed, and the reaction temperature is controlled to 87°C; when the acid value of the system is 38.4mgKOH / g, the esterification reaction ends;

[0065] (2) Cool down to 65°C and keep warm for 1h;

[0066] (3) The reaction system is cooled to 40° C., adding 10% of the acid value recorded in the organic phase, the excess concentration is 7% sodium hydroxide solution, 15% sodium chloride solution for neutralization, washing 2 times, and standing to take upper organic phase;

[0067] (4) After adding a concentration of 12% hydrochloric acid aqueous solution and a concentration of 15% sodium chloride solution for pickling and washing for 2 times, take the upper organic phase;

[0068] (5) adding 5% aqueous solution of sodium sulfite to the upper organic phase for decolorization treatment, and taking the upper organic p...

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Abstract

The invention discloses a preparation method of 1,3-glycerol diacrylate. The method comprises the following steps that glycerol, acrylic acid, polar solvents, catalysts, first polymerization inhibitors and chemical inhibitors are mixed, and the mixture passes through the air; when the acid value of the system is 15.4 to 49.82mgKOH / g, the esterification reaction is completed; the temperature is lowered to 60 to 70 DEG C; the heat insulation is performed for 1h; neutralization and washing are performed; acid is added for acid washing; after the washing, still standing layering is performed; the upper layer organic phase is taken; a water solution of a reducing agent is added into the upper layer organic phase to perform de-coloring treatment; a second polymerization inhibitor is added; solvents are removed from the upper layer organic phase; pressurization filtering is performed at 40 to 70 DEG C; a 1,3-glycerol diacrylate finished product is obtained. The preparation method has the advantages that the process is simple; the operation is convenient; the reaction terminal point can be easily controlled; the cost is low; the purity is very high.

Description

technical field [0001] The invention relates to the technical field of acrylate research, in particular to a preparation method of 1,3-propanetriol diacrylate. Background technique [0002] Acrylate is a general term for esters of acrylic acid and its homologues. The more important ones are methyl acrylate, ethyl acrylate, 2-methyl methacrylate and 2-ethyl methacrylate. It can be self-polymerized or copolymerized with other monomers, and it is a monomer for the manufacture of adhesives, synthetic resins, special rubber and plastics. [0003] According to the number of acrylphthalein groups (CHZ=CHCO-), acrylate monomers can be divided into monofunctional monomers, difunctional monomers and multifunctional monomers. Monofunctional monomer refers to a monomer with an acrylic group in its molecule, and the polymer formed after polymerization is a linear polymer without crosslinking. When using monofunctional monomers, it can not only increase the flexibility of the coating, ...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08C07C67/34
CPCC07C67/08C07C67/34C07C69/54
Inventor 钱保平谭鹏程为中吴泽光陈彬齐栋洋潘功礼查文平施戊辰
Owner ANQING FEIKAI NEW MATERIAL CO LTD
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