CN104892398A - Preparation method of mildew inhibitor - Google Patents
Preparation method of mildew inhibitor Download PDFInfo
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- CN104892398A CN104892398A CN201510273992.XA CN201510273992A CN104892398A CN 104892398 A CN104892398 A CN 104892398A CN 201510273992 A CN201510273992 A CN 201510273992A CN 104892398 A CN104892398 A CN 104892398A
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- inhibiting agent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
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Abstract
The invention discloses a preparation method of a mildew inhibitor. The preparation method comprises the following steps of a, weighing raw materials, namely anhydrous sodium acetate and acetic acid according to the molar ratio of 1:(1.000-1.050), adding the raw materials into a 250ml reaction vessel, adding anhydrous sodium acetate and 45% ethanol into the reaction vessel according to the weight ratio of 1:(0.80-1.0), stirring, and regulating the pH value to 4-5; b, reflowing in a water bath device for 2-2.5 hours to obtain a solution A; c, carrying out cooling crystallization on the solution A at the speed of 1.2-1.5 DEG C/min to obtain a solution B; d, filtering the solution B through a vacuum pump to obtain a solution C; and d, naturally drying the solution C, and packaging. The preparation method disclosed by the invention is convenient to operate, the yield of the mildew inhibitor is relatively high, the raw materials are available, and the sodium diacetate mildew inhibitor prepared by using the preparation method has a relatively-high economic benefit.
Description
Technical field
The present invention relates to the preparation process amelioration of mould inhibitor, specifically refer to a kind of preparation method of mould inhibiting agent.
Background technology
Grain goes mouldy and has a strong impact on quality product, causes the waste of resource, and the harm that grain goes mouldy has: grain caking produces the rotten quality that directly can affect grain, and then may cause larger financial loss because go mouldy.
Mould inhibiting agent main is at present sodium Diacetate, and its preparation method mainly contains aceticanhydride and sodium-acetate reaction method; Acetic acid and sodium hydroxide reaction method; Acetic acid or aceticanhydride and sodium carbonate reaction method and acetic acid-aceticanhydride and sodium carbonate reaction method; Acetic acid and sodium-acetate reaction method, except acetic acid and sodium-acetate reaction method production technique, although above-mentioned various method can obtain purer sodium Diacetate, but nearly all can relate to aceticanhydride, because the reaction times is longer, raw material aceticanhydride price is high, and yield is on the low side, and in the reaction process of sodium carbonate participation, also have a large amount of CO
2produce, therefore should not build technology device.
Summary of the invention
The object of the invention is to: the preparation method providing a kind of mould inhibiting agent, this preparation technology is simple, and raw material is easy to get, and cost is low, and the reaction times is short, and environmental protection is pollution-free, and the mould inhibiting agent product yield of preparation is higher.
The present invention is achieved through the following technical solutions as follows:
A preparation method for mould inhibiting agent, comprises the following steps:
A, take raw material, according to mol ratio anhydrous sodium acetate: acetic acid is 1:1.000-1.050, is added in 250ml reaction vessel, adds anhydrous sodium acetate and 45% ethanol in reaction vessel according to weight ratio 1:0.80-1.0, stir, and regulate PH to 4-5;
B, water bath device backflow 2h-2.5h, obtains solution A;
C, solution A, with the speed crystallisation by cooling of 1.2-1.5 DEG C/min, obtain solution B;
C, solution B to be filtered by vacuum pump, obtain solution C;
After d, solution C seasoning, pack and get final product.
Condensing reflux pipe is equipped with further, in order to better realize the present invention, described 250ml reaction vessel
Further, in order to better realize the present invention, in described step a, the mol ratio of anhydrous sodium acetate and acetic acid is 1:1.050.
Further, in order to better realize the present invention, the mother liquor of the solution B after filtering in described step C can be used as reaction solvent.
Further, in order to better realize the present invention, described reaction vessel is 250ml there-necked flask.
Further, in order to better realize the present invention, in described reaction vessel, the weight ratio of anhydrous sodium acetate and 45% ethanol is 1:0.80.
Further, in order to better realize the present invention, in described reaction vessel, the weight ratio of anhydrous sodium acetate and 45% ethanol is 1:1.0.
Further, in order to better realize the present invention, in described step C, the crystallization velocity of solution A is 1.2 DEG C/min.
Further, in order to better realize the present invention, in described step C, the crystallization velocity of solution A is 1.5 DEG C/min.
The present invention compared with prior art, has the following advantages and beneficial effect:
(1) mould inhibiting agent that obtains of preparation technology of the present invention, reaches through strict its quality that measures the international quality standards that Food and Argriculture OrganizationFAO and the World Health Organization specifies.
(2) preparation technology that takes of the present invention, not only technique is simple, easy to operate, and product yield is higher, and raw material is easy to get, and the mould inhibiting agent that this preparation technology obtains has higher economic benefit.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
A preparation method for mould inhibiting agent, comprises the following steps:
A, take raw material, according to mol ratio anhydrous sodium acetate: acetic acid is 1:1.000, is added in 250ml reaction vessel, adds anhydrous sodium acetate and 45% ethanol in reaction vessel according to weight ratio 1:0.80, stir, and regulate PH to 4.00;
B, water bath device backflow 2h, obtains solution A;
C, solution A, with the speed crystallisation by cooling of 1.2 DEG C/min, obtain solution B;
C, solution B to be filtered by vacuum pump, obtain solution C;
After d, solution C seasoning, pack and get final product.
Embodiment 2:
A, take raw material, according to mol ratio anhydrous sodium acetate: acetic acid is 1:1.030, is added in 250ml reaction vessel, adds anhydrous sodium acetate and 45% ethanol in reaction vessel according to weight ratio 1:0.90, stir, and regulate PH to 4.50;
B, refluxed by water bath device 2h, obtains solution A;
C, solution A, with the speed crystallisation by cooling of 1.3 DEG C/min, obtain solution B;
D, solution B vacuum pump to be filtered, obtain solution C;
After e, solution C seasoning, pack and get final product.
Embodiment 3:
A, take raw material, according to mol ratio anhydrous sodium acetate: acetic acid is 1:1.050, is added in 250ml reaction vessel, adds anhydrous sodium acetate and 45% ethanol in reaction vessel according to weight ratio 1:1.00, stir, and regulate PH to 5.00;
B, refluxed by water bath device 2.5h, obtains solution A;
C, solution A, with the speed crystallisation by cooling of 1.5 DEG C/min, obtain solution B;
D, solution B to be filtered by SH2-3 type water cycle vacuum pump, obtain solution C;
After e, solution C seasoning, pack and get final product.
Test portion:
Its Raw, anhydrous sodium acetate: industrial one-level, content is not less than 58%-60%, sodium carbonate: industrial one-level, content is not less than 98%.
Key instrument: SH2-3 type water cycle vacuum pump; The water bath with thermostatic control of HH-4 type digital display; JJ-1 type timing electric mixer; 250ml there-necked flask reactor; PHS-3C precision acidity meter; Q6110501 electro-heating standing-temperature cultivator.
---------dry---packaging---obtains sodium Diacetate product to crystallisation by cooling to sodium Diacetate synthesis flow: acetic acid and anhydrous sodium acetate carry out building-up reactions in filtration.
According to the best process flow determined, be equipped with in the 250ml there-necked flask of reflux condensing tube at one, add a certain amount of solvent, acetic acid and anhydrous sodium acetate by proportioning, heated and stirred, backflow for some time, crystallisation by cooling, filtration, drying, obtaining final product, the disposing mother liquor after filtration can be recycled.
Here the main ratio to sodium Diacetate preparation process Raw acetic acid and anhydrous sodium acetate is carried out preferably, realizes the quality and the yield that improve mould inhibiting agent.
Wherein acetic acid content is 45%, and consumption is 40g, and return time is 2h, and change the mol ratio of acetic acid and anhydrous sodium acetate, result is as table 1:
The impact of feed molar comparison product and yield
Can draw, when the mol ratio of control anhydrous sodium acetate and acetic acid is 1:1.000-1.050, more suitable.
On the basis of above-mentioned experiment, study further, the mol ratio selecting acetic acid and anhydrous sodium acetate is 1:1.050, and under the condition of backflow 2h, change the consumption of solvent, experimental result is as shown in table 2,
Solvent load is on the impact of quality product and yield
Can draw, the weight ratio of anhydrous sodium acetate and solvent 45% is that 1:0.0.8 is more suitable.
Further, in order to better realize the present invention, on above-mentioned basis, feed molar when when the condition such as solvent load is certain, changes the reaction times, the reaction times too short yield that can affect product, but after reaching certain hour, continue the reaction of propagation time, product yield is not made significant difference, show that the reaction times is that 2.0h is more suitable.
Further, in order to better realize the present invention, change the content of etoh solvent, the preferably ethanol of 45%, can be conducive to improving the quality of products further and product yield.As shown in table 3 below in detail:
From experimental result, select 45% ethanol as solvent, produce minimum, Recycling Mother Solution uses and product can be made to mention about 95% simultaneously, both reduces costs, and avoids again because discharge waste liquid causes the pollution to environment in a large number.
Anti-mold effect is tested
Mold species is aseptically inoculated on PDA solid medium, 10 days are cultivated in the temperature of 25 degree, spore is washed in aseptic aqueous solution, again by the spore suspension of 0.5ml with by above-mentioned preparation technology obtain 0.1% mould inhibiting agent sodium Diacetate solution fully mix after, be inoculated on PDA substratum, in even juxtaposition 30 degree of thermostat containers cultivate 96 days, observe colony growth situation, control group adopts the PDA not containing mould inhibitor dull and stereotyped, and bacteriostatic experiment result is as shown in table 4 below
Application mold test
The sample that test utilizes mould to breed with corn, bread, cake etc. carries out.Sample is divided into the test group adding mould inhibitor and the control group not adding mould inhibitor at random, and during test, get corn and bread respectively with after the sodium Diacetate even spraying of 1.00% and 0.05%, putting temperature is respectively 25 degree, cultivates in the incubator of relative humidity 85%.After one week, visual inspection test group mildew phenomena is obviously lighter than control group, its surface is in light yellow, maize germ portion can't see blackout situation, and control group is then in the majority with blackening person, and the mould inhibiting rate of food bread is also more than 90%, simultaneous test shows, New Type Antiseptic Germicide Sodium Diacetate can obviously grow by mould fungus inhibition, and the speed of growth of the mould that can slow down, has mildew-resistant and protect fresh effect.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls into protection scope of the present invention.
Claims (9)
1. a preparation method for mould inhibiting agent, is characterized in that, comprises the following steps:
A, take raw material, according to mol ratio anhydrous sodium acetate: acetic acid is 1:1.000-1.050, is added in 250ml reaction vessel, adds anhydrous sodium acetate and 45% ethanol in reaction vessel according to weight ratio 1:0.80-1.0, stir, and regulate PH to 4-5;
B, water bath device backflow 2h-2.5h, obtains solution A;
C, solution A, with 1.2-1.5 DEG C/min speed crystallisation by cooling, obtain solution B;
C, solution B to be filtered by vacuum pump, obtain solution C;
After d, solution C seasoning, pack and get final product.
2. the preparation method of a kind of mould inhibiting agent according to claim 1, is characterized in that: described 250ml reaction vessel is equipped with condensing reflux pipe.
3. the preparation method of a kind of mould inhibiting agent according to claim 2, is characterized in that: in described step a, the mol ratio of anhydrous sodium acetate and acetic acid is 1:1.050.
4. the preparation method of a kind of mould inhibiting agent according to claim 3, is characterized in that: the mother liquor of the solution B after filtering in described step C can be used as reaction solvent.
5. the preparation method of a kind of mould inhibiting agent according to claim 3, is characterized in that: described reaction vessel is 250ml there-necked flask.
6. the preparation method of a kind of mould inhibiting agent according to claim 4, is characterized in that: in described reaction vessel, the weight ratio of anhydrous sodium acetate and 45% ethanol is 1:0.80.
7. the preparation method of a kind of mould inhibiting agent according to claim 4, is characterized in that: in described reaction vessel, the weight ratio of anhydrous sodium acetate and 45% ethanol is 1:1.0.
8. the preparation method of a kind of mould inhibiting agent according to claim 5, is characterized in that: in described step C, the crystallization velocity of solution A is 1.2 DEG C/min.
9. the preparation method of a kind of mould inhibiting agent according to claim 6, is characterized in that: in described step C, the crystallization velocity of solution A is 1.5 DEG C/min.
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| CN201510273992.XA CN104892398A (en) | 2015-05-27 | 2015-05-27 | Preparation method of mildew inhibitor |
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| CN201510273992.XA CN104892398A (en) | 2015-05-27 | 2015-05-27 | Preparation method of mildew inhibitor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245031A (en) * | 2016-08-26 | 2017-10-13 | 南通奥凯生物技术开发有限公司 | A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531582A (en) * | 2009-01-06 | 2009-09-16 | 云南省玉溪市溶剂厂有限公司 | Method for preparing sodium diacetate by industrial waste |
| CN104496788A (en) * | 2014-11-27 | 2015-04-08 | 苏州嘉禧萝生物科技有限公司 | Preparation process of mould inhibitor |
| WO2015072494A1 (en) * | 2013-11-12 | 2015-05-21 | 扶桑薬品工業株式会社 | Novel sodium diacetate crystal and solid dialysis preparation comprising said crystal |
-
2015
- 2015-05-27 CN CN201510273992.XA patent/CN104892398A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531582A (en) * | 2009-01-06 | 2009-09-16 | 云南省玉溪市溶剂厂有限公司 | Method for preparing sodium diacetate by industrial waste |
| WO2015072494A1 (en) * | 2013-11-12 | 2015-05-21 | 扶桑薬品工業株式会社 | Novel sodium diacetate crystal and solid dialysis preparation comprising said crystal |
| CN104496788A (en) * | 2014-11-27 | 2015-04-08 | 苏州嘉禧萝生物科技有限公司 | Preparation process of mould inhibitor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245031A (en) * | 2016-08-26 | 2017-10-13 | 南通奥凯生物技术开发有限公司 | A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate |
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Application publication date: 20150909 Assignee: SICHAUN DICHEN AGRICULTURAL LIMITED LIABILITY COMPANY Assignor: Yi Chuansi bio tech ltd, Chengdu Contract record no.: 2016510000008 Denomination of invention: Preparation method of mildew inhibitor License type: Common License Record date: 20160506 |
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