CN108238928A - The process units of antibacterials 2,4- hexadiene acid - Google Patents

The process units of antibacterials 2,4- hexadiene acid Download PDF

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Publication number
CN108238928A
CN108238928A CN201710933672.1A CN201710933672A CN108238928A CN 108238928 A CN108238928 A CN 108238928A CN 201710933672 A CN201710933672 A CN 201710933672A CN 108238928 A CN108238928 A CN 108238928A
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CN
China
Prior art keywords
storage tank
reaction kettle
acid
process units
antibacterials
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201710933672.1A
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Chinese (zh)
Inventor
彭飞
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Chengdu Pollock Technology Co Ltd
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Chengdu Pollock Technology Co Ltd
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Application filed by Chengdu Pollock Technology Co Ltd filed Critical Chengdu Pollock Technology Co Ltd
Priority to CN201710933672.1A priority Critical patent/CN108238928A/en
Priority to GBGB1721085.7A priority patent/GB201721085D0/en
Publication of CN108238928A publication Critical patent/CN108238928A/en
Priority to AU2018101386A priority patent/AU2018101386A4/en
Withdrawn legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C57/00Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms
    • C07C57/02Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms with only carbon-to-carbon double bonds as unsaturation
    • C07C57/03Monocarboxylic acids
    • C07C57/10Sorbic acid
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/347Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
    • C07C51/377Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by splitting-off hydrogen or functional groups; by hydrogenolysis of functional groups
    • C07C51/38Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by splitting-off hydrogen or functional groups; by hydrogenolysis of functional groups by decarboxylation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The process units of 2,4 hexadiene acid of antibacterials, mainly includes:Storage tank 1 (F101), storage tank 2 (F102), storage tank 3 (F103), storage tank 4 (F104), condenser (C101), reaction kettle (D101), the connection relation between each component part of process units are:Storage tank 1 (F101) and storage tank 2 (F102) are connect side by side with reaction kettle (D101), storage tank 3 (F103) and storage tank 4 (F104) are connect side by side with reaction kettle (D101), and condenser (C101) is connect with reaction kettle (D101);Wherein, reaction kettle (D101) nominal volume is 300 350L;6 7mm of storage tank 1 (F101) cylinder wall thickness.

Description

The process units of antibacterials 2,4- hexadiene acid
Technical field
The present invention relates to pharmaceutical synthesis device more particularly to antibacterials 2, the process units of 4- hexadienes acid.
Background technology
2,4- hexadiene acid drugs are all inhibited to yeast, mould and many fungies, are that high effect nontoxic anti-corrosion is prevented Mould dose, for human food, animal feed, cosmetics, medicine, packaging material and rubber chemicals etc..Mould and ferment can be used as Inhibitor, antimildew agent for food, dryness oils denaturant, fungicide of female bacterium etc..2,4- hexadiene acid drugs can effectively inhibit The activity of mould, saccharomycete and aerobic bacteria, moreover it is possible to prevent the harmful microorganisms such as clostridium botulinum, staphylococcus, salmonella Growth and breeding, it is but nearly unavailable to the beneficial microbes such as anaerobic Bacillus and lactobacillus acidophilus, restrain the work of development With more stronger than bactericidal effect, so as to reach the holding time for effectively extending food, and the flavor of original food is kept.It is existing Process units is mostly more complicated, and therefore, 2,4- hexadiene acid are as antibacterials, and process units quality is for improving product Quality, reducing by-products content has Important Economic meaning.
Invention content
The purpose of the present invention is to provide antibacterials 2, the process units of 4- hexadienes acid mainly includes:Storage tank 1 (F101), storage tank 2 (F102), storage tank 3 (F103), storage tank 4 (F104), condenser (C101), reaction kettle (D101), process units Connection relation between each component part is:Storage tank 1 (F101) and storage tank 2 (F102) are connect side by side with reaction kettle (D101), Storage tank 3 (F103) and storage tank 4 (F104) are connect side by side with reaction kettle (D101), and condenser (C101) connects with reaction kettle (D101) It connects;Wherein, reaction kettle (D101) nominal volume is 300-350L;(F101) cylinder wall thickness of storage tank 1 6-7mm;Storage tank 2 (F102) seals Head thickness 8-10mm;Storage tank 3 (F103) cone base thickness degree 7-9mm.
Antibacterials 2, the process units of 4- hexadienes acid, production principle are crotonaldehyde and malonic acid in pyridine solvent Sorbic acid is obtained through decarboxylic reaction.Antibacterials 2, the process units of 4- hexadienes acid, production procedure are:Pyridine solvent is added in anti- It answers in kettle D101, adds crotonaldehyde and malonic acid, stir 2h at room temperature, be then to slowly warm up to 80 DEG C, maintain 60~70 DEG C Lower progress decarboxylic reaction 2-3h.Reaction finishes, and is cooled to 5 DEG C hereinafter, being slowly added into 10% dilute sulfuric acid, and temperature is controlled to be no more than 10 DEG C, until reactant is in faintly acid, pH is until 3-3.5.6h is cooled down, filtering, sorbic acid crude product is washed with water to obtain in solid, then uses 1-2 times of 40% ethyl alcohol recrystallize up to purified product.The invention has the advantages that:Reduce reaction intermediate link, reduce Reaction temperature and reaction time, improve reaction yield.
Description of the drawings
Fig. 1 is the process units figure of antibacterials 2,4- hexadiene acid.
Mainly include:Storage tank 1 (F101), storage tank 2 (F102), storage tank 3 (F103), storage tank 4 (F104), condenser (C101), reaction kettle (D101);
Specific embodiment
With reference to specific implementation example, the invention will be further described:
The process units of antibacterials 2,4- hexadiene acid
Example 1:
Raw materials for production and dosage
Antibacterials 2, the process units of 4- hexadienes acid, mainly include:Storage tank 1 (F101), storage tank 2 (F102), storage tank 3 (F103), storage tank 4 (F104), condenser (C101), reaction kettle (D101), the connection between each component part of process units are closed It is to be:Storage tank 1 (F101) and storage tank 2 (F102) are connect side by side with reaction kettle (D101), storage tank 3 (F103) and storage tank 4 (F104) It is connect side by side with reaction kettle (D101), condenser (C101) is connect with reaction kettle (D101);Wherein, reaction kettle (D101) nominal is held Product is 300L;(F101) cylinder wall thickness of storage tank 1 6mm;(F102) head thickness of storage tank 2 8mm;Storage tank 3 (F103) bores base thickness degree 7mm.Pyridine solvent is added in reaction kettle D101, crotonaldehyde and malonic acid is added, stirs 2h at room temperature, then slowly heating To 80 DEG C, maintain to carry out decarboxylic reaction 2h at 60 DEG C.Reaction finishes, and is cooled to 2 DEG C, is slowly added into 10% dilute sulfuric acid, and control 5 DEG C of temperature, until reactant is in faintly acid, pH is until 3.6h, filtering are cooled down, solid is washed with water to obtain sorbic acid crude product, then with 1 40% ethyl alcohol recrystallize up to purified product 2,4- hexadienes acid again.
Product 2,4- hexadiene acid quality is as follows:
Example 2:
Antibacterials 2, the process units of 4- hexadienes acid, mainly include:Storage tank 1 (F101), storage tank 2 (F102), storage tank 3 (F103), storage tank 4 (F104), condenser (C101), reaction kettle (D101), the connection between each component part of process units are closed It is to be:Storage tank 1 (F101) and storage tank 2 (F102) are connect side by side with reaction kettle (D101), storage tank 3 (F103) and storage tank 4 (F104) It is connect side by side with reaction kettle (D101), condenser (C101) is connect with reaction kettle (D101);Wherein, reaction kettle (D101) nominal is held Product is 350L;(F101) cylinder wall thickness of storage tank 1 7mm;(F102) head thickness of storage tank 2 10mm;Storage tank 3 (F103) bores base thickness degree 9mm.Pyridine solvent is added in reaction kettle D101, crotonaldehyde and malonic acid is added, stirs 3h at room temperature, then slowly heating To 70 DEG C, maintain to carry out decarboxylic reaction 3h at 65 DEG C.Reaction finishes, and is cooled to 3 DEG C, is slowly added into 15% dilute sulfuric acid, and control Temperature is no more than 6 DEG C, until reactant is in faintly acid, pH is until 3.5.Cool down 5h, filtering, solid be washed with water sorbic acid is thick Product, then with 2 times of 40% ethyl alcohol recrystallize up to purified product 2,4- hexadienes acid.
Product 2,4- hexadiene acid quality is as follows:
It described in above example, is merely preferred embodiments of the present invention, but protection scope of the present invention not office Be limited to this, any one skilled in the art in the technical scope disclosed by the present invention, the technique according to the invention Scheme and its inventive concept are subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (3)

1. antibacterials 2, the process units of 4- hexadienes acid, which is characterized in that mainly include:Storage tank 1 (F101), storage tank 2 (F102), storage tank 3 (F103), storage tank 4 (F104), condenser (C101), reaction kettle (D101), each component part of process units Between connection relation be:Storage tank 1 (F101) and storage tank 2 (F102) are connect side by side with reaction kettle (D101), storage tank 3 (F103) and Storage tank 4 (F104) is connect side by side with reaction kettle (D101), and condenser (C101) is connect with reaction kettle (D101);Wherein, reaction kettle (D101) nominal volume is 300-350L;(F101) cylinder wall thickness of storage tank 1 6-7mm.
2. antibacterials 2 according to claim 1, the process units of 4- hexadienes acid, which is characterized in that the storage tank 2 (F102) head thickness 8-10mm.
3. antibacterials 2 according to claim 1, the process units of 4- hexadienes acid, which is characterized in that the storage tank 3 (F103) cone base thickness degree 7-9mm.
CN201710933672.1A 2017-10-10 2017-10-10 The process units of antibacterials 2,4- hexadiene acid Withdrawn CN108238928A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201710933672.1A CN108238928A (en) 2017-10-10 2017-10-10 The process units of antibacterials 2,4- hexadiene acid
GBGB1721085.7A GB201721085D0 (en) 2017-10-10 2017-12-18 Antibacterial drug 2,4-hexadienic acid production
AU2018101386A AU2018101386A4 (en) 2017-10-10 2018-09-21 Antibacterial drug 2,4-hexadienic acid production plant

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710933672.1A CN108238928A (en) 2017-10-10 2017-10-10 The process units of antibacterials 2,4- hexadiene acid

Publications (1)

Publication Number Publication Date
CN108238928A true CN108238928A (en) 2018-07-03

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CN201710933672.1A Withdrawn CN108238928A (en) 2017-10-10 2017-10-10 The process units of antibacterials 2,4- hexadiene acid

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CN (1) CN108238928A (en)
AU (1) AU2018101386A4 (en)
GB (1) GB201721085D0 (en)

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GB201721085D0 (en) 2018-01-31
AU2018101386A4 (en) 2018-10-25

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