CN107245031A - A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate - Google Patents
A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate Download PDFInfo
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- CN107245031A CN107245031A CN201610739440.8A CN201610739440A CN107245031A CN 107245031 A CN107245031 A CN 107245031A CN 201610739440 A CN201610739440 A CN 201610739440A CN 107245031 A CN107245031 A CN 107245031A
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- sodium acetate
- anhydrous sodium
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- mould inhibitor
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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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Abstract
, should comprising the following steps that by the preparation method of the obtained mould inhibitor of anhydrous sodium acetate the invention discloses a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate of the preparation method technical field of mould inhibitor：S1：Choose raw material；S2：Heating and thermal insulation；S3：Crystallisation by cooling；S4：Filtering crystals；S5：Heating distillation；S6：Dehydration；S7：Detection, storage, the preparation method of mould inhibitor is made by anhydrous sodium acetate for this, using anhydrous sodium acetate as producing raw material, reaction time is relatively short, price is relatively low, efficiency is higher, avoid the shortcoming that sodium carbonate preparation method produces great amount of carbon dioxide, by the way of secondary filter, the large granular impurity in raw material is crossed into elimination first, the fine particulate filter in solution is removed using milipore filter, it is incubated using water-bath, the change of water-bath holding temperature is smaller, and the influence to reaction product is smaller, helpful for preparing result success rate.
Description
Technical field
It is specially that one kind is made mould by anhydrous sodium acetate the present invention relates to the preparation method technical field of mould inhibitor
The preparation method of bacteria inhibitor.
Background technology
Mould inhibitor main at present is sodium Diacetate, and its preparation method mainly has 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
With sodium acetate reaction method, in addition to acetic acid and sodium acetate reaction method production technology, although above-mentioned various methods can obtain purer
Sodium Diacetate, but can nearly all be related to aceticanhydride, because the reaction time is longer, raw material aceticanhydride price is high, and yield is relatively low, Er Qie
In the course of reaction that sodium carbonate is participated in, also substantial amounts of carbon dioxide is produced, therefore should not build technology device, such as Chinese
A kind of preparation technology of mould inhibitor of special example Application No. 201410707843.5, comprises the following steps, a, according to anhydrous second
Sour sodium and acetic acid mol ratio is 1:1.005-1.035 weigh raw material, add to the 250ml reaction vessels that reflux condenser is housed
In, according to sodium acetate and 45% ethanol weight ratio 1 in reaction vessel：0.75-1.1 add, stirring, and adjust PH；B, pass through water
Bath apparatus backflow 1.5h -2h, obtains solution A；C, solution A obtain solution B with 1.5-1.8 DEG C/min speed crystallisation by cooling；
C, solution B is filtered by SH2-3 type water circulation vavuum pumps, obtain solution C；After d, solution C are spontaneously dried, packaging is
, mould inhibitor purity prepared by this kind of method is not high enough, therefore, being made mould by anhydrous sodium acetate we have proposed one kind
The preparation method of bacteria inhibitor.
The content of the invention
It is an object of the invention to provide a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate, to solve
The existing method reaction time for preparing mould inhibitor proposed in above-mentioned background technology is longer, and raw material aceticanhydride price is high, receives
The problem of rate is relatively low.
To achieve the above object, the present invention provides following technical scheme：It is a kind of that mould suppression is made by anhydrous sodium acetate
The preparation method of agent, should comprising the following steps that by the preparation method of the obtained mould inhibitor of anhydrous sodium acetate：
S1：Choose raw material：Mass ratio from anhydrous sodium acetate and acetic acid is 8.2：(6.03-6.21), is placed in anti-
Answer in container, ethanol is added into reaction vessel, the ratio between ethanol and anhydrous sodium acetate are (6.15-9.02)：8.2, and stir extremely
Solid is completely dissolved；
S2：Heating and thermal insulation：Reaction vessel in acquisition step S1, and the solution in reaction vessel is heated, the heat time
For 10 minutes, it is incubated after heating；
S3：Crystallisation by cooling：Reaction vessel after being incubated in step S2 is placed in cooling chamber, the temperature of cooling chamber gradually under
Drop, the decrease speed for setting temperature is 1.2-1.6 centigrade per minutes, separates out crystal；
S4：Filtering crystals：The reaction vessel that cooling in step S3 is separated out into crystal is taken out and filtered using sieves,
Solution after filtering is subjected to secondary filter by milipore filter, the solution after filtering is deposited using clean beaker；
S5：Heating distillation：The beaker for having solution after filtering in obtaining step S4, distillation is placed in by the solution in beaker
Distill, crystallize in tower；
S6：Dehydration：Crystal after being distilled in acquisition step S5 in destilling tower, cooling, the crystal after cooling adds dewaterer
In, obtain the solid powder after dehydration；
S7：Detection, storage：Solid powder after being dehydrated in step S6 is obtained and detected, the article after detection uses close
Seal container to preserve, and sealing container is placed in hothouse memory storage.
It is preferred that, the reaction vessel in the step S1 is round-bottomed flask, and the side wall of round-bottomed flask has condensing reflux
Pipe.
It is preferred that, the concentration of the ethanol added in the step S1 is 40-50%, and the pH value of solution is 4-5.
It is preferred that, the heating-up temperature of the step S2 is 65-80 degrees Celsius, and the time of insulation is 2-2.5 hours.
It is preferred that, the mode of heating in the step S2 is heated using microwave, and heat preserving mode is incubated using water-bath.
It is preferred that, the cut off that crystal is separated out in the step S3 is：When temperature continues to decline the body of crystal in five minutes
Product no longer changes, you can terminate cooling step.
It is preferred that, the distillation time in the step S5 is 3-4 hours, and the vapo(u)rizing temperature in destilling tower is taken the photograph for 100-120
Family name's degree.
It is preferred that, the cool time in the step S6 is 30-35 minutes, and dewatering time is 10-15 minutes.
It is preferred that, atmospheric water content is 5-8% in hothouse in the step S7, and the temperature 5-10 in hothouse takes the photograph
Family name's degree.
Compared with prior art, the beneficial effects of the invention are as follows：The system of mould inhibitor is made by anhydrous sodium acetate for this
Preparation Method, using anhydrous sodium acetate as producing, raw material, reaction time are relatively short, and price is relatively low, and efficiency is higher, it is to avoid
Sodium carbonate preparation method produces the shortcoming of great amount of carbon dioxide, by the way of secondary filter, first by big in raw material
Grain contaminant filter is gone, and is removed the fine particulate filter in solution using milipore filter, is incubated using water-bath, the change of water-bath holding temperature
Smaller, the influence to reaction product is smaller, helpful for preparing result success rate.
Brief description of the drawings
Fig. 1 is mould inhibitor preparation flow figure of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment one
Referring to Fig. 1, the present invention provides a kind of technical scheme：A kind of system that mould inhibitor is made by anhydrous sodium acetate
Preparation Method, should comprising the following steps that by the preparation method of the obtained mould inhibitor of anhydrous sodium acetate：
S1：Choose raw material：Mass ratio from anhydrous sodium acetate and acetic acid is 8.2：6.03, it is placed in reaction vessel
In, ethanol is added into reaction vessel, the ratio between ethanol and anhydrous sodium acetate are 6.15：8.2, and stir to solid and be completely dissolved,
Reaction vessel is round-bottomed flask, and the side wall of round-bottomed flask has condensing reflux pipe, and the concentration of ethanol is 40%, and the PH of solution
It is worth for 4；
S2：Heating and thermal insulation：Reaction vessel in acquisition step S1, and the solution in reaction vessel is heated, the heat time
For 10 minutes, it is incubated after heating, heating-up temperature is 65 degrees Celsius, the time of insulation is 2 hours, and mode of heating is added using microwave
Heat, heat preserving mode is incubated using water-bath；
S3：Crystallisation by cooling：Reaction vessel after being incubated in step S2 is placed in cooling chamber, the temperature of cooling chamber gradually under
Drop, the decrease speed for setting temperature is 1.2 centigrade per minutes, separates out crystal, when temperature continues to decline crystal in five minutes
Volume no longer changes, you can terminate cooling step；
S4：Filtering crystals：The reaction vessel that cooling in step S3 is separated out into crystal is taken out and filtered using sieves,
Solution after filtering is subjected to secondary filter by milipore filter, the solution after filtering is deposited using clean beaker；
S5：Heating distillation：The beaker for having solution after filtering in obtaining step S4, distillation is placed in by the solution in beaker
Distill, crystallize in tower, distillation time is 3 hours, the vapo(u)rizing temperature in destilling tower is 100 degrees Celsius；
S6：Dehydration：Crystal after being distilled in acquisition step S5 in destilling tower, cooling, the crystal after cooling adds dewaterer
In, the solid powder after dehydration is obtained, cool time is 30 minutes, and dewatering time is 10 minutes；
S7：Detection, storage：Solid powder after being dehydrated in step S6 is obtained and detected, the article after detection uses close
Container is sealed to preserve, and it is in 5%, hothouse that sealing container is placed in into atmospheric water content in hothouse memory storage, hothouse
5 degrees Celsius of temperature.
Embodiment two
A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate, should be made mould by anhydrous sodium acetate and press down
The preparation method of preparation is comprised the following steps that：
S1：Choose raw material：Mass ratio from anhydrous sodium acetate and acetic acid is 8.2：6.12, it is placed in reaction vessel
In, ethanol is added into reaction vessel, the ratio between ethanol and anhydrous sodium acetate are 7.58：8.2, and stir to solid and be completely dissolved,
Reaction vessel is round-bottomed flask, and the side wall of round-bottomed flask has condensing reflux pipe, and the concentration of ethanol is 45%, and the PH of solution
It is worth for 4.5；
S2：Heating and thermal insulation：Reaction vessel in acquisition step S1, and the solution in reaction vessel is heated, the heat time
For 10 minutes, it is incubated after heating, heating-up temperature is 72 degrees Celsius, the time of insulation is 2.3 hours, and mode of heating is added using microwave
Heat, heat preserving mode is incubated using water-bath；
S3：Crystallisation by cooling：Reaction vessel after being incubated in step S2 is placed in cooling chamber, the temperature of cooling chamber gradually under
Drop, the decrease speed for setting temperature is 1.35 centigrade per minutes, separates out crystal, when temperature continues to decline crystal in five minutes
Volume no longer changes, you can terminate cooling step；
S4：Filtering crystals：The reaction vessel that cooling in step S3 is separated out into crystal is taken out and filtered using sieves,
Solution after filtering is subjected to secondary filter by milipore filter, the solution after filtering is deposited using clean beaker；
S5：Heating distillation：The beaker for having solution after filtering in obtaining step S4, distillation is placed in by the solution in beaker
Distill, crystallize in tower, distillation time is 3.5 hours, the vapo(u)rizing temperature in destilling tower is 110 degrees Celsius；
S6：Dehydration：Crystal after being distilled in acquisition step S5 in destilling tower, cooling, the crystal after cooling adds dewaterer
In, the solid powder after dehydration is obtained, cool time is 33 minutes, and dewatering time is 13 minutes；
S7：Detection, storage：Solid powder after being dehydrated in step S6 is obtained and detected, the article after detection uses close
Container is sealed to preserve, and it is 6.5%, hothouse that sealing container is placed in into atmospheric water content in hothouse memory storage, hothouse
7.5 degrees Celsius of interior temperature.
Embodiment three
A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate, should be made mould by anhydrous sodium acetate and press down
The preparation method of preparation is comprised the following steps that：
S1：Choose raw material：Mass ratio from anhydrous sodium acetate and acetic acid is 8.2：6.21, it is placed in reaction vessel
In, ethanol is added into reaction vessel, the ratio between ethanol and anhydrous sodium acetate are 9.02：8.2, and stir to solid and be completely dissolved,
Reaction vessel is round-bottomed flask, and the side wall of round-bottomed flask has condensing reflux pipe, and the concentration of ethanol is 50%, and the PH of solution
It is worth for 5；
S2：Heating and thermal insulation：Reaction vessel in acquisition step S1, and the solution in reaction vessel is heated, the heat time
For 10 minutes, it is incubated after heating, heating-up temperature is 80 degrees Celsius, the time of insulation is 2.5 hours, and mode of heating is added using microwave
Heat, heat preserving mode is incubated using water-bath；
S3：Crystallisation by cooling：Reaction vessel after being incubated in step S2 is placed in cooling chamber, the temperature of cooling chamber gradually under
Drop, the decrease speed for setting temperature is 1.6 centigrade per minutes, separates out crystal, when temperature continues to decline crystal in five minutes
Volume no longer changes, you can terminate cooling step；
S4：Filtering crystals：The reaction vessel that cooling in step S3 is separated out into crystal is taken out and filtered using sieves,
Solution after filtering is subjected to secondary filter by milipore filter, the solution after filtering is deposited using clean beaker；
S5：Heating distillation：The beaker for having solution after filtering in obtaining step S4, distillation is placed in by the solution in beaker
Distill, crystallize in tower, distillation time is 4 hours, the vapo(u)rizing temperature in destilling tower is 120 degrees Celsius；
S6：Dehydration：Crystal after being distilled in acquisition step S5 in destilling tower, cooling, the crystal after cooling adds dewaterer
In, the solid powder after dehydration is obtained, cool time is 35 minutes, and dewatering time is 15 minutes；
S7：Detection, storage：Solid powder after being dehydrated in step S6 is obtained and detected, the article after detection uses close
Container is sealed to preserve, and it is in 8%, hothouse that sealing container is placed in into atmospheric water content in hothouse memory storage, hothouse
10 degrees Celsius of temperature.
According to the experimental result of above example one, two, three, most preferred embodiment is embodiment two.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (9)
1. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate, it is characterised in that：Anhydrous sodium acetate should be passed through
The preparation method that mould inhibitor is made is comprised the following steps that：
S1：Choose raw material：Mass ratio from anhydrous sodium acetate and acetic acid is 8.2：(6.03-6.21), is placed in reaction and holds
In device, ethanol is added into reaction vessel, the ratio between ethanol and anhydrous sodium acetate are (6.15-9.02)：8.2, and stir to solid
It is completely dissolved；
S2：Heating and thermal insulation：Reaction vessel in acquisition step S1, and the solution in reaction vessel is heated, the heat time is 10
Minute, it is incubated after heating；
S3：Crystallisation by cooling：Reaction vessel after being incubated in step S2 is placed in cooling chamber, the temperature of cooling chamber is gradually reduced, if
The decrease speed for putting temperature is 1.2-1.6 centigrade per minutes, separates out crystal；
S4：Filtering crystals：The reaction vessel that cooling in step S3 is separated out into crystal is taken out and filtered using sieves, incited somebody to action
Solution after filter carries out secondary filter by milipore filter, and the solution after filtering is deposited using clean beaker；
S5：Heating distillation：The beaker for having solution after filtering in obtaining step S4, the solution in beaker is placed in destilling tower
Distillation, crystallization；
S6：Dehydration：Crystal after being distilled in acquisition step S5 in destilling tower, cooling, the crystal after cooling is added in dewaterer, is taken
Solid powder after must being dehydrated；
S7：Detection, storage：Solid powder after being dehydrated in step S6 is obtained and detected, the article after detection is held using sealing
Device is preserved, and sealing container is placed in into hothouse memory storage.
2. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：Reaction vessel in the step S1 is round-bottomed flask, and the side wall of round-bottomed flask has condensing reflux pipe.
3. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：The concentration of the ethanol added in the step S1 is 40-50%, and the pH value of solution is 4-5.
4. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：The heating-up temperature of the step S2 is 65-80 degrees Celsius, and the time of insulation is 2-2.5 hours.
5. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：Mode of heating in the step S2 is heated using microwave, and heat preserving mode is incubated using water-bath.
6. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：The cut off of precipitation crystal is in the step S3：No longer change when temperature continues to decline the volume of crystal in five minutes, i.e.,
Cooling step can be terminated.
7. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：Distillation time in the step S5 is 3-4 hours, and the vapo(u)rizing temperature in destilling tower is 100-120 degrees Celsius.
8. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：Cool time in the step S6 is 30-35 minutes, and dewatering time is 10-15 minutes.
9. a kind of preparation method that mould inhibitor is made by anhydrous sodium acetate according to claim 1, its feature exists
In：Atmospheric water content is the temperature in 5-8%, hothouse for 5-10 degrees Celsius in hothouse in the step S7.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610739440.8A CN107245031A (en) | 2016-08-26 | 2016-08-26 | A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate |
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| CN201610739440.8A CN107245031A (en) | 2016-08-26 | 2016-08-26 | A kind of preparation method that mould inhibitor is made by anhydrous sodium acetate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114983990A (en) * | 2022-08-01 | 2022-09-02 | 广州康盛生物科技股份有限公司 | Stable glacial acetic acid-sodium acetate compound and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735032A (en) * | 2008-11-04 | 2010-06-16 | 唐玉量 | Method for preparing sodium diacetate |
| 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 |
| CN104892398A (en) * | 2015-05-27 | 2015-09-09 | 成都易创思生物科技有限公司 | Preparation method of mildew inhibitor |
-
2016
- 2016-08-26 CN CN201610739440.8A patent/CN107245031A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735032A (en) * | 2008-11-04 | 2010-06-16 | 唐玉量 | Method for preparing sodium diacetate |
| 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 |
| CN104892398A (en) * | 2015-05-27 | 2015-09-09 | 成都易创思生物科技有限公司 | Preparation method of mildew inhibitor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114983990A (en) * | 2022-08-01 | 2022-09-02 | 广州康盛生物科技股份有限公司 | Stable glacial acetic acid-sodium acetate compound and application thereof |
| CN114983990B (en) * | 2022-08-01 | 2022-10-28 | 广州康盛生物科技股份有限公司 | Stable glacial acetic acid-sodium acetate compound and application thereof |
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Application publication date: 20171013 |