Ethephon solid purification method

A purification method and ethephon technology, applied in the field of ethephon solid purification, can solve the problems of difficult crystallization of solvents, difficult to obtain products, influence on product yield and purity stability, etc., and achieve the effects of less pollution and avoiding low-temperature operation.

Active Publication Date: 2018-04-10
孟州农达生化制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually in the production of ethephon, due to insufficient raw material purity, improper control of material ratio and process conditions, side reactions will increase, resulting in increased by-products, which will greatly affect the stability of product yield and purity, and seriously affect the export volume of products.
The existing reported ethephon purification technology mainly has the following problems: the one is that the acid anhydride content cannot be effectively reduced, especially the results of comparing acid-base titration and gas chromatography to detect the purity of ethephon products are quite different. It shows that there are many acid anhydrides in the impurities; the second is that it is difficult to obtain high-purity ethephon powder products. Due to the strong water absorption of ethephon, it is difficult to crystallize in general solvents, even if a large amount of ether is used as a solvent for a long time at a very low temperature for a long time to crystallize , and only a small amount of ethephon solid can be obtained, and powdered ethephon products are even more difficult to obtain

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0021] Example 1: Take 300g of industrial product ethephon with a mass content of 85% in a 1500mL beaker, add 900mL of water, stir to dissolve and leave it overnight; after extraction with 90mL of cyclohexane, use a rotary evaporator to evaporate the water to obtain crude ethephon; Use a Soxhlet extractor to cyclically extract the crude ethephon with 300 mL of dichloroethane and acetone in a volume ratio of 2:1 as a mixed solvent, and the cyclic extraction time is 7.5 hours; the obtained solution is again used to evaporate the mixed solvent with a rotary evaporator. 220.8 g of white powder with 94.3% purity of ethephon was obtained, and the yield was 73.6%.

Embodiment 2

[0022] Example 2: Take 300g of industrial product ethephon solids with 85% mass content in a 1500mL beaker, add 900mL of water, stir to dissolve and leave overnight; after extraction with 90mL of acetone, use a rotary evaporator to evaporate the water to obtain crude ethephon; Use a Soxhlet extractor to circulate and extract the crude ethephon with 300mL of dichloroethane and acetone in a volume ratio of 2:1 as solvents. The cyclic extraction time is 7 hours; after obtaining the solution, use the rotary evaporator to evaporate the mixed solvent again to obtain The purity is 93.6% ethephon white powder 222.6g, and the yield is 74.2%.

Embodiment 3

[0023] Example 3: Take 300 g of industrial product ethephon with a mass content of 85% in a 1500 mL beaker, add 900 mL of water, stir to dissolve and leave it overnight; after extraction with 90 mL of dichloromethane, use a rotary evaporator to evaporate the water to obtain crude ethephon; Use a Soxhlet extractor to circulate and extract the crude ethephon with 300mL of dichloroethane and acetone in a volume ratio of 2:1 as solvents. The cyclic extraction time is 6 hours; after obtaining the solution, use the rotary evaporator to evaporate the mixed solvent again to obtain The purity is 226.5g of 92.8% ethephon white powder, and the yield is 75.5%.

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Abstract

The invention discloses an ethephon solid purification method. Powdery high-purity ethephon product are obtained at normal temperature by applying a combined operation mode of hydrolysis, extraction, primary rotary evaporation, mixed solvent continuous extraction and secondary rotary evaporation on ethephon which is an industrial product. The ethephon solid purification method particularly includes: using water to dissolve ethephon which is the industrial product of 85% in mass content, and placing overnight after stirring for dissolving; after organic solvent extraction, applying a rotary evaporation instrument to evaporate water out to obtain a crude ethephon product; applying a Soxhlet extractor to circularly extract the crude ethephon product by using dichloroethane and acetone as mixed extracting agents to obtain a solution, and applying the rotary evaporation instrument to evaporate dichloroethane and acetone out to obtain white ethephon powder exceeding 92.8% in content and exceeding 73.1% in yield. Mass powdery high-purity ethephon products are obtained at the normal temperature, so that inorganic and organic impurities are removed effectively, low-temperature operation is avoided, and the ethephon solid purification method causes little pollution, saves energy, protects environment and has industrial application prospect.

Description

Technical field [0001] The invention specifically relates to a method for purifying ethephon solids. Background technique [0002] Ethephon (chloroethyl phosphonic acid) is a plant growth regulator. When the pH value is greater than 3, ethylene can be slowly released, and the residue is non-toxic and harmless phosphate. Ethylene is an excellent plant growth regulator. It plays an important role in the growth process of seed germination, plant growth, flowering and fruit maturation, tissue senescence and shedding. In addition, when plants are subjected to harsh environmental stress, pests and diseases or mechanical damage, ethylene can respond quickly and enhance various resistances of plants. However, because ethylene is often a gaseous substance, it cannot be used directly in the field and outdoors, which greatly limits the application of ethylene in plants. The synthesis of ethylene provides the possibility for the application of ethylene in plants. The pH value of plant tiss...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
CPCC07F9/3808
Inventor 韦长梅支三军蒋正静
Owner 孟州农达生化制品有限公司
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