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Post-treatment method of homocystine reaction solution

A technology of homocystine and reaction solution, applied in chemical instruments and methods, sulfur trioxide/sulfuric acid, preparation of organic compounds, etc., can solve the problems of incomplete recovery of acid, high cost, complicated dialysis recovery device, etc.

Active Publication Date: 2020-09-08
九江中星医药化工有限公司
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  • Abstract
  • Description
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Problems solved by technology

Chinese patent CN101348452A discloses a method for preparing homocystine from methionine and sulfuric acid / hydrohalic acid. The post-treatment method of the reaction solution is to dialysis the reaction solution to recover excess sulfuric acid, which greatly reduces the waste salt. However, due to the concentration of counter ions in dialysis, the excess acid in the reaction solution cannot be completely recovered in production, and the dialysis recovery device is complicated and costly

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  • Post-treatment method of homocystine reaction solution
  • Post-treatment method of homocystine reaction solution

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Experimental program
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Effect test

Embodiment 1

[0051] Methionine (50.0g, 0.37mol) and hydrobromic acid (180.6g, mass percent concentration 47%, 1.05mol) were stirred and mixed evenly at room temperature, and concentrated sulfuric acid (68.0g, mass percent concentration 98% , 0.68mol) and stirred evenly, then hydrothermal co-reacted at 130°C for 13h to obtain a homocystine reaction solution (300mL);

[0052] according to figure 1 The post-treatment method of the homocystine reaction solution shown, after cooling the homocystine reaction solution to room temperature, add 300mL pure water for dilution, and place the gained diluted reaction solution (injection volume is 600mL) in a strong After adsorption in the ion-exchange column of acidic cation exchange resin (model Dowex-50 H type, the resin amount is 500.0g), once eluted with pure water until no sulfuric acid and hydrobromic acid are washed out, water eluent is obtained; water The eluate was recovered after vacuum distillation to obtain mixed acid (hydrochloric acid and...

Embodiment 2

[0056] Methionine (50.0g, 0.37mol) and hydrobromic acid (160.1g, mass percent concentration 47%, 0.93mol) were stirred at room temperature, and concentrated sulfuric acid (80.0g, 0.80mol) was added dropwise and stirred evenly, and then Hydrothermal co-reaction at 125°C for 8 hours to obtain a homocystine reaction solution (about 300 mL);

[0057] After the homocystine reaction solution was cooled to room temperature, 500 mL of pure water was added to dilute it, and the resulting diluted reaction solution (injection volume was 800 mL) was placed in a strongly acidic cation exchange resin (model Amberlite IR-120 H type, resin Amount is 500.0g) after adsorbing in the ion-exchange column, carry out once-elution to ion-exchange column with pure water to no sulfuric acid and hydrobromic acid wash-out, obtain water eluate; Water eluate is after vacuum distillation Recover mixed acid (sulfuric acid and hydrobromic acid solution, mixed acid yield is 97%);

[0058] Utilize 15wt% dilute...

Embodiment 3

[0060] Methionine (50.0g, 0.37mol) and hydrobromic acid (223.8g, mass percent concentration 47%, 1.30mol) were stirred at room temperature, and concentrated sulfuric acid (80.0g, mass percent concentration 98%, 0.80 mol) was stirred evenly, and then hydrothermally co-reacted at 125°C for 8h to obtain a homocystine reaction solution (about 300mL);

[0061] After the homocystine reaction solution is cooled to room temperature, add 500mL of pure water for dilution, and the diluted reaction solution (injection volume: 800mL) is placed in a place filled with a strongly acidic cation exchange resin (model Dowex-650C H type, resin volume 500.0g) after adsorption in the ion-exchange column, the ion-exchange column is eluted once with pure water until no sulfuric acid and hydrobromic acid are washed out to obtain the water eluate; the water eluate is recovered after vacuum distillation Obtain mixed acid (sulfuric acid and hydrobromic acid, mixed acid yield is 97%);

[0062] Use 10wt% ...

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Abstract

The invention provides a post-treatment method of a homocystine reaction solution, and relates to the technical field of homocystine preparation. The post-treatment method of the homocystine reactionsolution comprises the following steps: adsorbing the homocystine reaction solution in acid ion exchange resin, performing primary elution on the adsorption ion exchange resin through water, obtainingeluent and deacidified ion exchange resin, and wherein the eluent comprises recycled sulfuric acid and hydrobromic acid; and carrying out secondary elution on the deacidified ion exchange resin by using an acid eluent or an alkali eluent to obtain an acid eluent or an alkali eluent, the acid eluent or the alkali eluent containing homocystine. According to the post-treatment method, sulfuric acidand hydrobromic acid are weak in adsorption capacity in acidic ion resin, and are easily eluted with water to be separated from the reaction solution so that a large amount of waste salt generated byneutralizing the reaction liquid with alkali liquor is avoided, and the method is green and environment-friendly; complex devices are not needed, and the cost is low.

Description

technical field [0001] The invention relates to the technical field of preparation of homocystine, in particular to a post-treatment method of homocystine reaction liquid. Background technique [0002] Homocysteine ​​and its reductive cyclization product (homocysteine ​​thiolactone hydrochloride) are important pharmaceutical and pesticide intermediates. The structural formula of homocysteine ​​is as follows: [0003] [0004] The literature J.Biol.chem, 1999; 135-142 first proposed the synthesis method of homocystine: heating methionine and excess sulfuric acid to prepare homocysteine. This method has been used until now, but the reaction yield is low, and later During the treatment process, alkaline solution is used to neutralize excess sulfuric acid, which produces a large amount of inorganic salts, causing great pressure on environmental protection. European patent EP0844239 has improved the above method: homocystine is prepared by heating methionine and sulfuric acid...

Claims

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Application Information

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IPC IPC(8): C07C319/24C07C319/28C07C323/58C01B7/09C01B17/90
CPCC07C319/24C07C319/28C01B7/093C01B17/90C07C323/58
Inventor 骆建轻周以鸿何文秀程龙进周建雄赖立冬
Owner 九江中星医药化工有限公司
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