CN105646192A - Acetylchloride decoloring method - Google Patents
Acetylchloride decoloring method Download PDFInfo
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- CN105646192A CN105646192A CN201610167844.4A CN201610167844A CN105646192A CN 105646192 A CN105646192 A CN 105646192A CN 201610167844 A CN201610167844 A CN 201610167844A CN 105646192 A CN105646192 A CN 105646192A
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- acetyl chloride
- chloride 98min
- acetylchloride
- decoloring method
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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
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/64—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention discloses an acetylchloride decoloring method, relating to the field of organic matter decoloring. The method comprises the following steps: preparing peracetic acid with the concentration of 3.5-9.8 percent; according to parts by mass, adding at least 5 parts of the peracetic acid into 100 parts of color-changed acetylchloride; after stirring uniformly, increasing temperature to be not higher than 80 DEG C, and rectifying until cutoff. By deeply analyzing impurities in the acetylchloride, a matter resulting in the color change of the acetylchloride is determined to be ethenone; the organic matter resulting in the color change in the acetylchloride is removed by the peracetic acid; while the acetylchloride is purified, color change of the acetylchloride is prevented, thus improving the use value of the acetylchloride.
Description
Technical field
The present invention relates to organism decolouring field, it is specifically related to a kind of Acetyl Chloride 98Min. decoloring method.
Background technology
The process of industrial use acetic anhydride and METHYL TRICHLORO SILANE Reactive Synthesis methyl triacetoxysilane can generate by product Acetyl Chloride 98Min..
Acetyl Chloride 98Min. as organic synthesis raw material, for the production of agricultural chemicals, medicine, Novel electroplating complexing agent, the catalyzer of carboxylic acid generation chlorination reaction, acetylize reagent and other multiple Minute Organic Synthesis intermediates.
Owing to also having the existence of other side reactions in process of production, depositing with, in transportation, trace impurity character is unstable with the Acetyl Chloride 98Min. of the active organism of character, causing the color of Acetyl Chloride 98Min. to become dark.
Current Acetyl Chloride 98Min. is about 7 days from the colourless time length turned within the scope of the distinguishable color of naked eyes, if accumulating temperature is too high, when color changes, length can be shorter.
Occur in the Acetyl Chloride 98Min. of variable color containing trace impurity, and after the Acetyl Chloride 98Min. of variable color is carried out purification again and rectifying, the later stage deposit with transportation in still can there is variable color, not only affect outward appearance, and the reaction that Acetyl Chloride 98Min. participates in can be had an impact by impurity, it is unfavorable for that it is as the normal use of reaction raw materials in various field, downstream, at present, owing to Acetyl Chloride 98Min. itself is relatively more active, usually adopting gac it to be decoloured, effect is poor.
Summary of the invention
For the defect existed in prior art, it is an object of the invention to provide a kind of Acetyl Chloride 98Min. decoloring method, the organism more active containing unsaturated link(age) and character in Acetyl Chloride 98Min. can be removed, effectively prevent Acetyl Chloride 98Min. variable color in transporting and depositing, it is to increase the use value of Acetyl Chloride 98Min..
For reaching above object, the technical scheme that the present invention takes is:
A kind of Acetyl Chloride 98Min. decoloring method, comprises the following steps:
Preparation concentration is the Peracetic Acid of 3.5��9.8%, by mass parts, adds at least 5 parts of Peracetic Acids in the Acetyl Chloride 98Min. of 100 parts of variable colors, is warming up to and does not carry out rectifying to cutout higher than 80 DEG C after stirring evenly.
On the basis of technique scheme, described middle preparation concentration be 3.5��9.8% Peracetic Acid comprise the following steps: in flask, drop into aceticanhydride, heat up 40 DEG C��50 DEG C, at the uniform velocity drip under agitation and add the hydrogen peroxide that concentration is 20��35%, the mass ratio of hydrogen peroxide and aceticanhydride is 1:7��12, stirring the obtained destainer of 40��100min, described destainer is CH3COOOH��
On the basis of technique scheme, the concentration of described hydrogen peroxide is 30%.
On the basis of technique scheme, the mass ratio of described hydrogen peroxide and aceticanhydride is 1:10.
On the basis of technique scheme, the rate of addition of described hydrogen peroxide is 2��4g/min.
On the basis of technique scheme, the churning time of described obtained destainer is 60min.
On the basis of technique scheme, in described step B, the temperature of rectifying is 60��80 DEG C.
On the basis of technique scheme, described step B comprises the following steps: by mass parts, adds at least 5 parts of destainers in the Acetyl Chloride 98Min. of 100 parts of variable colors, is warming up to 65 DEG C and carries out rectifying to cutout after stirring evenly.
A kind of Peracetic Acid, described Peracetic Acid is for decolouring to Acetyl Chloride 98Min..
Compared with prior art, it is an advantage of the current invention that:
(1) the Acetyl Chloride 98Min. decoloring method in the present invention, by the impurity in Acetyl Chloride 98Min. is analysed in depth, the material determining to cause Acetyl Chloride 98Min. variable color is ketene, and remove the organism causing variable color in Acetyl Chloride 98Min. by Peracetic Acid, while Acetyl Chloride 98Min. is carried out purifying, prevent Acetyl Chloride 98Min. two variable colors, it is to increase the use value of Acetyl Chloride 98Min..
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
The embodiment of the present invention provides a kind of Acetyl Chloride 98Min. decoloring method, comprises the following steps:
A, preparation concentration is the Peracetic Acid (in the present embodiment of 3.5��9.8%, the concentration of Peracetic Acid is 6.1%), in actual use, the concentration of Peracetic Acid can be 4.5��8.0%, 5.0��7.5% or 6.0��7%, flask drops into aceticanhydride, after being warming up to 40 DEG C, it is 40 DEG C��50 DEG C (optimum is 45 DEG C) in temperature, it is that 2��4g/min drips and adds the hydrogen peroxide that mass concentration is 20��35% (optimum is 30%) according to speed under stirring, the mass ratio of hydrogen peroxide and aceticanhydride is that 1:7��12 are (in the present embodiment, the mass ratio of hydrogen peroxide and aceticanhydride is 1:10), stir the obtained destainer of 40��100min (optimum is 1h), destainer is CH3COOOH��
B, by mass parts, at least 5 parts of destainers are added in the Acetyl Chloride 98Min. of 100 parts of variable colors, the rectifying when temperature is no more than 80 DEG C, in the present embodiment, when temperature is 60 DEG C��70 DEG C (optimum is 65 DEG C), keep at the uniform velocity rectifying, evaporate after point output speed slows down and slowly heat up, it is being no more than in 80 DEG C of situations, till evaporating cutout. Reaction mechanism is roughly as follows:
(CH3CO)2O+H2O2��CH3COOOH (Peracetic Acid, destainer effective constituent)+CH3COOH;
(CH3CO)2O+H2O��2CH3COOH (destainer by product);
2CH3COOOH��2CH3COOH+O2(destainer decomposition mechanism);
CH3Unstable target compound �� the stable in properties of COOOH+ character and colourless organism.
At present, cannot consider about the concrete color products storing generation in Acetyl Chloride 98Min., the present invention is by analyzing the side reaction involved by all reactants and reaction product, through inferring that reaction raw materials acetic anhydride decomposes in high temperature production process, the ketene of generation is the composition easily causing variable color and being difficult to remove.
But owing to the Acetyl Chloride 98Min. purity of industrial production is generally more than 98%, wherein also containing other impurity, and the content of ketene is very few, it is difficult to the detection methods by routine (such as gas-chromatography, liquid chromatography, mass spectrum etc.) and judges whether the material causing variable color is ketene, therefore, the industry fail always preferably solve this problem of Acetyl Chloride 98Min. variable color.
When producing Acetyl Chloride 98Min., due to the boiling point of acetic acid be 117.9 DEG C, the boiling point of METHYL TRICHLORO SILANE be 66.5 DEG C, the boiling point of methyl triacetoxysilane be 141��143 DEG C, all higher than the boiling point 51 DEG C of Acetyl Chloride 98Min., therefore, can by distillation mode, obtain low temperature fraction Acetyl Chloride 98Min., and due to the boiling point of Acetyl Chloride 98Min. lower, therefore, it is possible to by the mode of rectifying, Acetyl Chloride 98Min. is carried out purifying;But, owing to the boiling point of ketene is-56 DEG C, it is gas at normal temperatures, when being obtained by the mode of distillation or during purifying Acetyl Chloride 98Min., ketene can be inevitable enter in Acetyl Chloride 98Min., and ketene can be dissolved in Acetyl Chloride 98Min., namely Acetyl Chloride 98Min. can remain the ketene residual of trace, also it is difficult to remove through repeatedly rectifying.
It is that 0.2��0.5% (this scope obtains according to test of many times result for contriver that the present invention adds mass ratio in the Acetyl Chloride 98Min. that purity is 99%, within the scope of other all can not with the mating mutually of control group) ketene as experimental group, by existing by product Acetyl Chloride 98Min. as a control group, using purity be 99% Acetyl Chloride 98Min. as blank group, carry out when other conditions are all identical depositing (or transport), the variable color time and the color that obtain experimental group and control group are basically identical, and blank group does not have variable color, the variable color that the reason causing Acetyl Chloride 98Min. variable color is impurity ketene can be estimated according to this test.
Owing to Peracetic Acid with ketene, following reaction can occur: ketene+Peracetic Acid=acetic anhydride, acetic anhydride is isolated in Acetyl Chloride 98Min. system by rectification process, therefore, the present invention removes the ketene in Acetyl Chloride 98Min. according to the mechanism of this reaction, although the mechanism of reaction is fairly simple, but the present invention just determines to cause the reason of variable color by long-time research with after exploring, it not simply consult the result that document just can obtain the present invention.
To those skilled in the art, it is once black that the standard of Acetyl Chloride 98Min. variable color is that the colourity of solution is greater than 30, and existing Acetyl Chloride 98Min. stores and in transportation, and the colourity after usually storing a week is 50��60 once black.
It is described in detail below by 6 specific embodiments.
Embodiment 1
Disposable input aceticanhydride 200g in 500ml there-necked flask, warming while stirring, treat that temperature is raised to about 40 DEG C, start to drip with dropping funnel that to add 20g mass concentration be 30% hydrogen peroxide, keep the rate of addition of 2��4g/min at the uniform velocity to drip to add, drip and add in process control temperature at 40 DEG C��50 DEG C, obtained destainer after at the uniform velocity stirring 1h.
The Acetyl Chloride 98Min. 200g of disposable input variable color in 500ml there-necked flask and 10g destainer, set 65 DEG C, start to heat up and stir rectifying, extraction in early stage evaporates point may be quicker, starting to heat up after evaporating point comparison on rate of yield limit slowly, temperature-rise period should not be too fast, when being no more than 80 DEG C, rectifying is to cutout, and point sealing that evaporates of collection preserves.
Embodiment 2
The operation steps of the present embodiment is substantially the same manner as Example 1, and difference is as follows: the mass concentration dripping the hydrogen peroxide added is 20%, and aceticanhydride and hydrogen peroxide mass ratio are 7:1, and the quality of the destainer added is 20g.
Embodiment 3
The operation steps of the present embodiment is substantially the same manner as Example 1, and difference is as follows: the mass concentration dripping the hydrogen peroxide added is 35%, and aceticanhydride and hydrogen peroxide mass ratio are 12:1, and the quality of the destainer added is 18g.
Embodiment 4
The operation steps of the present embodiment is substantially the same manner as Example 1, and difference is as follows: the quality of the destainer added is 15g.
Embodiment 5
The operation steps of the present embodiment is substantially the same manner as Example 1, and difference is as follows: the destainer quality added is 5g.
Embodiment 6
The operation steps of the present embodiment is substantially the same manner as Example 1, and difference is as follows: the destainer quality added is 0g.
Embodiment 7
The operation steps of the present embodiment is substantially the same manner as Example 1, and difference is as follows: the reaction times of hydrogen peroxide and aceticanhydride is 40min.
Embodiment 8
The operation steps of the present embodiment is substantially the same manner as Example 1, and difference is as follows: the reaction times of hydrogen peroxide and aceticanhydride is 100min.
The Acetyl Chloride 98Min. purifying obtained after being processed by embodiment 1 to 6 is colourless transparent liquid, above-mentioned four Acetyl Chloride 98Min. purification of samples are placed in experimental group, control group and blank group, at identical conditions, place after 7 days, all have there is macroscopic variable color in embodiment 5 and embodiment 6, wherein, the color of embodiment 5 is 45 once black, and it is once black that the appearance color when the 30th day of the sample in embodiment 6 turns into 30; Have there is macroscopic variable color after storing 15 days in embodiment 3 and embodiment 4; There is extremely slight variable color after storing 2 months in embodiment 7 and embodiment 8; Embodiment 1 and the sample in embodiment 2 appearance color after storing 3 months does not still change, thus known, when the mass ratio of Acetyl Chloride 98Min. and destainer is more than or equal to 20:1, there is good decolorizing effect, considering from maximization of economic benefit, the optimum proportion of variable color Acetyl Chloride 98Min. and destainer is 20:1.
The present invention also provides a kind of Peracetic Acid, and this Peracetic Acid is for decolouring to Acetyl Chloride 98Min..
The present invention is not limited to above-mentioned enforcement mode, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, and these improvements and modifications are also considered as within protection scope of the present invention. The content not being described in detail in this specification sheets belongs to the known prior art of professional and technical personnel in the field.
Claims (9)
1. an Acetyl Chloride 98Min. decoloring method, it is characterised in that: comprise the following steps:
Preparation concentration is the Peracetic Acid of 3.5��9.8%, by mass parts, adds at least 5 parts of Peracetic Acids in the Acetyl Chloride 98Min. of 100 parts of variable colors, is warming up to and does not carry out rectifying to cutout higher than 80 DEG C after stirring evenly.
2. a kind of Acetyl Chloride 98Min. decoloring method as claimed in claim 1, it is characterized in that: described middle preparation concentration be 3.5��9.8% Peracetic Acid comprise the following steps: in flask, drop into aceticanhydride, heat up 40 DEG C��50 DEG C, at the uniform velocity drip under agitation and add the hydrogen peroxide that concentration is 20��35%, the mass ratio of hydrogen peroxide and aceticanhydride is 1:7��12, stirring the obtained destainer of 40��100min, described destainer is CH3COOOH��
3. a kind of Acetyl Chloride 98Min. decoloring method as claimed in claim 2, it is characterised in that: the concentration of described hydrogen peroxide is 30%.
4. a kind of Acetyl Chloride 98Min. decoloring method as claimed in claim 3, it is characterised in that: the mass ratio of described hydrogen peroxide and aceticanhydride is 1:10.
5. a kind of Acetyl Chloride 98Min. decoloring method as claimed in claim 2, it is characterised in that: the rate of addition of described hydrogen peroxide is 2��4g/min.
6. a kind of Acetyl Chloride 98Min. decoloring method as claimed in claim 2, it is characterised in that: the churning time of described obtained destainer is 60min.
7. a kind of Acetyl Chloride 98Min. decoloring method as claimed in claim 1, it is characterised in that: in described step B, the temperature of rectifying is 60��80 DEG C.
8. a kind of Acetyl Chloride 98Min. decoloring method as claimed in claim 7, it is characterised in that: described step B comprises the following steps: by mass parts, adds at least 5 parts of destainers in the Acetyl Chloride 98Min. of 100 parts of variable colors, is warming up to 65 DEG C and carries out rectifying to cutout after stirring evenly.
9. a Peracetic Acid, it is characterised in that: described Peracetic Acid is for decolouring to Acetyl Chloride 98Min..
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610167844.4A CN105646192B (en) | 2016-03-22 | 2016-03-22 | A kind of chloroacetic chloride discoloration method |
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| CN201610167844.4A CN105646192B (en) | 2016-03-22 | 2016-03-22 | A kind of chloroacetic chloride discoloration method |
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| CN105646192B CN105646192B (en) | 2018-03-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108117487A (en) * | 2017-12-27 | 2018-06-05 | 湖北新蓝天新材料股份有限公司 | The application of chloroacetic chloride discoloration method and acid strong oxidizer in chloroacetic chloride decoloration |
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| SU458541A1 (en) * | 1972-06-08 | 1975-01-30 | Сумгаитский Филиал Ордена Трудового Красного Знамени Института Нефтехимических Процессов Им.Акад.Ю.Г.Мамедалиева | Acetyl Chloride Production Method |
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| CN104262440A (en) * | 2014-09-10 | 2015-01-07 | 江西赣亮医药原料有限公司 | Preparation method of 16alpha-hydroxyprednisolone |
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2016
- 2016-03-22 CN CN201610167844.4A patent/CN105646192B/en active Active
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| SU458541A1 (en) * | 1972-06-08 | 1975-01-30 | Сумгаитский Филиал Ордена Трудового Красного Знамени Института Нефтехимических Процессов Им.Акад.Ю.Г.Мамедалиева | Acetyl Chloride Production Method |
| JPS56127329A (en) * | 1980-03-10 | 1981-10-06 | Daicel Chem Ind Ltd | Preparation of monochloroacetic acid |
| CN101921289A (en) * | 2010-08-23 | 2010-12-22 | 湖北新蓝天新材料股份有限公司 | Method for producing methyltriacetoxysilane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108117487A (en) * | 2017-12-27 | 2018-06-05 | 湖北新蓝天新材料股份有限公司 | The application of chloroacetic chloride discoloration method and acid strong oxidizer in chloroacetic chloride decoloration |
| CN108117487B (en) * | 2017-12-27 | 2021-01-05 | 湖北新蓝天新材料股份有限公司 | Acetyl chloride decoloring method and application of acidic strong oxidant in acetyl chloride decoloring |
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| CN105646192B (en) | 2018-03-06 |
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