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Method for continuously preparing glutaraldehyde

A technology of glutaraldehyde and dihydropyran, which is applied in the field of synthetic methods and devices of chemical products, can solve the problems of slow reaction speed, high impurity content, long reaction time, etc., and achieves mild reaction conditions, simple equipment structure, no The effect of stirring energy

Active Publication Date: 2015-03-04
湖北微控生物科技有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] In method one, since the hydrolysis of alkoxydihydropyran is a reversible reaction, if methanol is not separated during the reaction, the alkoxydihydropyran cannot be completely converted, resulting in a low reaction yield in this method, and using a solid acid catalyst lead to slow reaction rate and more by-products
In the second method, the reaction time in the rectification tower is long, the energy consumption is high, the reaction is not complete, and the product has high impurity content
In the third method, the hydrolysis reaction takes a long time, and the refining and purification process is complex and contains many impurities, the refining pressure is high, and the total yield of the method is low
The above methods all have problems such as low yield, long residence time of materials, adjustment of product concentration and pH value, etc.
Specifically, due to the active chemical properties of glutaraldehyde, thermal instability, instability at high concentrations, instability of the pH value of the aqueous solution exceeding 2.5-5.0, and easy polymerization and yellowing of the color, the products produced by the above method contain 1 ~16% of by-products such as methanol, 2~5% of alkoxydihydropyran and glutaraldehyde polymers and other impurities cannot be directly used in the fields of medical sanitation, disinfection and scientific research

Method used

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  • Method for continuously preparing glutaraldehyde
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Experimental program
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Effect test

Embodiment 1

[0031] The static mixer that the embodiment of the present invention adopts is SV-3.5 / 32 type, and the tubular reactor volume is 0.2m 3 , the diameter of the rectification tower is Φ600, and the filling specification of the rectification tower is Dn25 SO 4 2- / TiO 2 -AL 2 o 3 -Al solid acid Raschig ring catalytic rectification filler 9m (this filler is equivalent to 2~2.5 theoretical plates per meter), of which, the rectification section is 5m, and the stripping section is 4m.

[0032] First, feed 2-methoxy-3,4-dihydropyran 800kg / h, water 960kg / h and phosphoric acid 0.5kg / h into the static mixer; In a tubular reactor, it is hydrolyzed at 95°C and 1.0Mpa (the residence time is about 6 minutes based on the feed volume and the volume of the tubular reactor). The hydrolysis conversion of 2-methoxy-3,4-dihydropyran after partial hydrolysis was 86%.

[0033] Secondly, the hydrolyzate after partial hydrolysis in the tubular reactor is passed into the rectification tower, and th...

Embodiment 2

[0036] First of all, this embodiment adopts the device in Embodiment 1 and the production process is the same, 600 kg / h of 2-methoxy-3,4-dihydropyran, 760 kg / h of water and 0.35 kg of phosphoric acid are introduced into the static mixer / h. In a tubular reactor, hydrolyze at 80°C and 0.3Mpa (the residence time is about 9 minutes according to the volume of the feed and the volume of the tubular reactor), after partial hydrolysis, 2-methoxy-3,4- The hydrolysis conversion rate of dihydropyran was 89%.

[0037] Secondly, in the reactive distillation process, the reactive distillation conditions are as follows: the pressure at the top of the tower is 46KPa, the temperature at the bottom of the tower is 86°C, and the reflux ratio is 0.7.

[0038] Finally, 349.9kg / h distillate was obtained from the top of the tower, among which, methanol 165.7kg / h, glutaraldehyde 6kg / h, 2-methoxy-3,4-dihydropyran 2.5kg / h and water 167.7 kg / h. Obtain glutaraldehyde finished product from the bottom ...

Embodiment 3

[0040] The static mixer that the embodiment of the present invention adopts is SV-2.3 / 20 type, and the tubular reactor volume is 0.15m 3 , the diameter of the rectification tower is Φ450, the packing is bagged β-zeolite 16m (each meter of this packing is equivalent to 1 theoretical plate), among them, the rectification section is 10m, and the stripping section is 6m.

[0041] First, feed 2-methoxy-3,4-dihydropyran 300kg / h, water 400kg / h and phosphoric acid 0.2kg / h into the static mixer; In a type reactor, it is hydrolyzed at 75°C and 0.2Mpa (the residence time is about 13 minutes based on the feed volume and the volume of the tubular reactor). The hydrolysis conversion rate of 2-methoxy-3,4-dihydropyran after partial hydrolysis was 90%.

[0042] Secondly, the hydrolyzate after partial hydrolysis in the tubular reactor is passed into the rectification tower, and the reaction rectification conditions are as follows: the pressure at the top of the tower is 33KPa, the temperature...

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Abstract

The invention discloses a method and a device for continuously preparing glutaraldehyde and belongs to the field of synthesis of chemical products. The method comprises the following steps of: fully mixing water, 2-methoxy-3,4-dihydropyran and phosphoric acid, partially hydrolyzing the 2-methoxy-3,4-dihydropyran in a tubular reactor, wherein the mass ratio of the water to 2-methoxy-3,4-dihydropyran to phosphoric acid is 1000-10000:1500-2500:1 during partial hydrolysis; adding the product of partial hydrolysis into a rectifying tower filled with a solid acid catalyst, reacting and rectifying, so that the 2-methoxy-3,4-dihydropyran is completely hydrolyzed; and removing the by-product methanol, thus obtaining the finished glutaraldehyde product. According to the method and the device, 2-methoxy-3,4-dihydropyran serves as a raw material, high-purity glutaraldehyde is prepared through partial hydrolysis, reaction and rectification; the glutaraldehyde is high in yield, high in purity, almost does not have impurities; and the cost is low and blending operation is omitted.

Description

technical field [0001] The invention relates to the field of synthetic methods and devices for chemical products, in particular to a method for continuously preparing glutaraldehyde, in particular to a continuous production method for high-purity glutaraldehyde that can be directly used in the fields of medical treatment and scientific research. Background technique [0002] Glutaraldehyde is an excellent fungicide, disinfectant, leather tanning agent, tissue curing agent, protein crosslinking agent, etc. Widely used in industrial water treatment, sanitation and disinfection, petrochemical industry, paper industry, leather tanning and scientific research fields; it is an important chemical intermediate and fine chemical product. The production of glutaraldehyde in the prior art basically adopts the hydrolysis method of 2-methoxyl-3,4-dihydropyran, and usually the following three methods can be used to obtain glutaraldehyde: [0003] Method one, discloses a kind of preparati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/12C07C45/60C07C45/82
Inventor 赵立群
Owner 湖北微控生物科技有限公司
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