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Glutaraldehyde preparation method

A technology for glutaraldehyde and acrolein, which is applied in the field of preparing glutaraldehyde by hydrolysis of 2-methoxy-3.4-dihydropyran under negative pressure, can solve the problem that glutaraldehyde solution is easy to change color, cannot be continuously produced, and equipment is anti-corrosion. High requirements for problems, to achieve the effects of high product quality stability, short reaction time, and improved utilization

Inactive Publication Date: 2018-04-13
濮阳盛华德化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] JP7226488, US2546018 announced the synthesis of glutaraldehyde with phosphoric acid or alkyl dibasic acid as a catalyst. The reaction conditions are mild and the yield is high, but the requirements for equipment anticorrosion are high. After the reaction, the catalyst remains in the system and the glutaraldehyde solution is easy to change color. And easily produce polycondensation deterioration; EP0717026, US7709686 and CN1233610 have reported the use of solid acid catalyst hydrolysis 2-methoxy-3.4-dihydropyran synthesis glutaraldehyde, solid acid comprises acidic resin, heteropoly acid etc., although this method overcomes It overcomes the disadvantage that the liquid acid corrosion equipment catalyst is difficult to separate, and the conversion rate of pyran is also high, but the resin is expensive and easily swells and deforms, which increases the production cost
US5679868, CN1709573 have released the method that uses zeolite as catalyst hydrolysis dihydropyran, although this method conversion rate is higher, but the hydrolysis time of this reaction is too long and cannot carry out continuous production; CN1371348A has reported a kind of glutaraldehyde continuous hydrolysis method, but the catalyst and reaction conditions are not described in detail, and the reaction speed is slow

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  • Glutaraldehyde preparation method

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Embodiment 1

[0024] A method for preparing glutaraldehyde, which uses acetylene, methanol, and acrolein as raw materials to prepare 2-methoxy-3.4-dihydropyran, and then hydrolyzes 2-methoxy-3.4-dihydropyran under negative pressure to prepare Glutaraldehyde, described preparation method comprises the following steps:

[0025] a. Synthesis of vinyl methyl ether: In a pressure vessel, under the conditions of 135°C and an absolute pressure of 0.5Mpa, methanol and acetylene are catalyzed by alkali metal salts of methanol to generate vinyl methyl ether;

[0026] b. Synthesis of pyran: In a reaction vessel, under the conditions of 130°C and an absolute pressure of 3.5Mpa, react acrolein with vinyl methyl ether for 2 hours to generate 2-methoxy-3.4-dihydropyran;

[0027] c. Purification of glutaraldehyde by hydrolysis of pyran: In a tubular reactor, under the condition of 70°C, 2-methoxy-3.4-dihydropyran is mixed with deionized water and then added with a polymerization inhibitor. Under the actio...

Embodiment 2

[0038] A method for preparing glutaraldehyde, which uses acetylene, methanol, and acrolein as raw materials to prepare 2-methoxy-3.4-dihydropyran, and then hydrolyzes 2-methoxy-3.4-dihydropyran under negative pressure to prepare Glutaraldehyde, described preparation method comprises the following steps:

[0039] a. Synthesis of vinyl methyl ether: In a pressure vessel, under the conditions of 140°C and an absolute pressure of 0.6Mpa, methanol and acetylene are catalyzed by alkali metal salts of methanol to generate vinyl methyl ether;

[0040] b. Synthesis of pyran: In a reaction vessel, under the conditions of 140°C and an absolute pressure of 4Mpa, acrolein and vinyl methyl ether are reacted to generate 2-methoxy-3.4-dihydropyran;

[0041] c. Purification of glutaraldehyde by hydrolyzing pyran: In a tubular reactor, mix 2-methoxy-3.4-dihydropyran with deionized water at 79°C and add a polymerization inhibitor, under the catalysis of strong acid resin Carry out pre-reaction ...

Embodiment 3

[0053] A method for preparing glutaraldehyde, which uses acetylene, methanol, and acrolein as raw materials to prepare 2-methoxy-3.4-dihydropyran, and then hydrolyzes 2-methoxy-3.4-dihydropyran under negative pressure to prepare Glutaraldehyde, described preparation method comprises the following steps:

[0054] a. Synthesis of vinyl methyl ether: In a pressure vessel, under the conditions of 130°C and an absolute pressure of 0.4Mpa, methanol and acetylene are catalyzed by alkali metal salts of methanol to generate vinyl methyl ether;

[0055] b. Synthesis of pyran: In a reaction vessel, under the conditions of 150°C and an absolute pressure of 3Mpa, acrolein and vinyl methyl ether are reacted to generate 2-methoxy-3.4-dihydropyran;

[0056] c. Purification of glutaraldehyde by hydrolyzing pyran: In a tubular reactor, under the conditions of 75°C and an absolute pressure of 0.05Mpa, add a polymerization inhibitor after mixing 2-methoxy-3.4-dihydropyran with deionized water , ...

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Abstract

The invention discloses a glutaraldehyde preparation method. Glutaraldehyde is prepared by using acetylene, methanol and acraldehyde as raw materials to produce and prepare 2-methoxy-3.4 dihydropyranand hydrolyzing 2-methoxy-3.4 dihydropyran under negative pressure to prepare glutaraldehyde. The method includes following steps: a, synthesizing vinyl methyl ether; b, synthesizing pyran; c, hydrolyzing pyran to purify glutaraldehyde. Generally, the method has the advantages of high reaction conversion rate, long catalyst service life, mild reaction condition, simplicity and convenience in operation, supportiveness of continuous production, high product purity, little environment pollution and extremely high practical value.

Description

technical field [0001] The invention belongs to the field of synthetic methods of chemical products, and relates to a method for preparing glutaraldehyde by hydrolyzing 2-methoxy-3.4-dihydropyran under negative pressure. Background technique [0002] Glutaraldehyde is an important saturated linear fatty cluster dialdehyde, which is widely used in petroleum exploration, medical and health, biochemistry, leather tanning agent, protein crosslinking agent, biological enzyme, food, cosmetics and other fields. At present, the synthesis methods of glutaraldehyde mainly include pyridine method, pentanediol oxidation method, reduction method, pyran method, and cyclopentene oxidation method. Glutadioxime is decomposed by sodium nitrite and hydrochloric acid to obtain glutaraldehyde. This method has a long process route, large consumption, large pollution, and high cost. It is not suitable for production and use; pentanediol oxidation method, the oxidation depth of this reaction is not...

Claims

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Application Information

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IPC IPC(8): C07C45/60C07C47/12C07C45/86C07C45/78C07C41/08C07C43/16C07D309/30
CPCC07C41/08C07C45/60C07C45/78C07C45/86C07D309/30C07C47/12C07C43/16
Inventor 王书生孙维华陈全胜李德彪
Owner 濮阳盛华德化工有限公司
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