CN105129734A - Method for recovering available substances in chloroacetic acid production tail gas - Google Patents
Method for recovering available substances in chloroacetic acid production tail gas Download PDFInfo
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- CN105129734A CN105129734A CN201510451831.5A CN201510451831A CN105129734A CN 105129734 A CN105129734 A CN 105129734A CN 201510451831 A CN201510451831 A CN 201510451831A CN 105129734 A CN105129734 A CN 105129734A
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- hydrochloric acid
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Abstract
The invention discloses a method for recovering available substances in chloroacetic acid production tail gas. The method comprises that low-boiling point substances are recovered from hydrogen chloride by a gradient condensation method, the low-boiling point substances are fully washed by dilute hydrochloric acid so that acetyl chloride and chloroacetyl chloride in hydrogen chloride gas, acetic acid and water in the dilute hydrochloric acid undergo a reaction, the reduced acetic acid and chloroacetic acid participate in the reaction again, and the hydrogen chloride gas subjected to impurity removal is subjected to cyclic absorption under the action of purified water in a clean absorption device, wherein in the absorption process, dissolving heat is taken away, so that high-quality refined hydrochloric acid with purity of 99.9% or more is obtained. Through a lot of experiments, the method for recovering available substances in chloroacetic acid production tail gas is selected. The method has a reasonable whole technical design, small equipment investment, low energy consumption and production process control easiness. The hydrochloric acid product has good quality, purity of 99.9% or more and a high usage value. The method realizes change of waste into valuables, reduces a production cost and has an important application value.
Description
Technical field
The present invention relates to a kind of preparation method of chemical reagent, be specifically related to a kind of steady quality, technique is controlled, reclaims the method for the utilized material in production of chloroacetic acid tail gas.
Technical background
In production of chloroacetic acid, the mechanism of the reaction of chlorine and acetic acid is, chlorine and catalyzer form the intermediate product of rare alcohol of formula structure, and this intermediate product is unstable, with acetic acidreaction, generate Acetyl Chloride 98Min., chloroacetyl chloride, chloroacetyl chloride again with acetic acidreaction, generate Mono Chloro Acetic Acid, produce hydrogen chloride gas in reaction process, absorb with water, prepare hydrochloric acid.
Carry a certain amount of Acetyl Chloride 98Min. secretly, chloroacetyl chloride, the intermediate products such as acetic acid in hydrogen chloride gas due to generation, not only affect the quality of hydrochloric acid, the intermediate product of simultaneous reactions can not change into product, and add raw-material consumption, the wasting of resources, cost is higher.Therefore necessaryly process tail gas hydrogenchloride, reclaim intermediate product, prepare the refining hydrochloric acid that industrial value is high, conservation, reduces costs.
Summary of the invention
Goal of the invention: the object of the invention is the deficiency existed to solve prior art, there is provided a kind of technological design reasonable, steady quality, energy consumption is low, fully can remove the Acetyl Chloride 98Min. in hydrogen chloride gas, chloroacetyl chloride, the intermediate products such as acetic acid, make full use of the method that the tail gas preparation of hydrogen chloride producing Mono Chloro Acetic Acid generation obtains high purity extractive salt manufacturing acid.
Technical scheme: in order to realize above object, the technical scheme that the present invention takes is:
Reclaim a method for the utilized material in production of chloroacetic acid tail gas, it is characterized in that, comprise the following steps:
(1) tail gas produced Mono Chloro Acetic Acid and produce is got, first reclaim through-10 ~-15 DEG C of condensations and obtain low-boiling point material, and then obtaining low-boiling point material through-20 ~-30 DEG C of condensations recovery, merging is reclaimed the low-boiling point material obtained and is continued transported to reactive system continuation reaction;
(2) step (1) condensed hydrogen chloride gas is got, be passed into volume tank and adopt dilute hydrochloric acid washing absorption, make the Acetyl Chloride 98Min. in hydrogen chloride gas, chloroacetyl chloride, water in acetic acid and dilute hydrochloric acid reacts, be reduced into acetic acid and Mono Chloro Acetic Acid, when in the dilute hydrochloric acid in volume tank, moisture content reaches after below 1%, this washings continues reaction as raw material input response system; Washing tank continues to change dilute hydrochloric acid and remakes washings;
(3) get the hydrogen chloride gas after step (2) washing, absorb at clean absorption equipment internal recycle by purified water;
(4) remove solution heat in absorption process, prepare the refining hydrochloric acid of purity more than 99.9%.
Preferably, the method of the utilized material in above-described recovery production of chloroacetic acid tail gas, step (1) gets the tail gas produced Mono Chloro Acetic Acid and produce, first reclaim through-15 DEG C of condensations and obtain low-boiling point material, and then obtaining low-boiling point material through-30 DEG C of condensations recovery, merging is reclaimed the low-boiling point material obtained and is continued transported to reactive system continuation reaction.Described low-boiling point material is Acetyl Chloride 98Min., chloroacetyl chloride and acetic acid.The present invention is screened by great many of experiments, preferably obtains best gradient and to cool impurity-removing method.
Preferably, the method for the utilized material in above-described recovery production of chloroacetic acid tail gas, step (2) washing adopt dilute hydrochloric acid be volume dense be 10% ~ 30% hydrochloric acid.
Preferably, the method for the utilized material in above-described recovery production of chloroacetic acid tail gas, removes solution heat with less than 10 DEG C water coolants in step (5).
Compared to the prior art, the present invention has the following advantages:
The present invention screens the method for the utilized material in the recovery production of chloroacetic acid tail gas obtained by great many of experiments, whole technological design is reasonable, facility investment is little, energy consumption is low, production process is easy to control, low-boiling point material is reclaimed by gradient freezing method, fully wash with dilute hydrochloric acid again, make the Acetyl Chloride 98Min. in hydrogen chloride gas, chloroacetyl chloride, water in acetic acid and dilute hydrochloric acid reacts, be reduced into acetic acid and Mono Chloro Acetic Acid and again participate in reaction, the high-quality hydrochloric acid of the high purity more than 99.9% prepared, use value is high, the present invention is turned waste into wealth, the input of raw material can be reduced, reduce production cost, there is important using value.
Specific implementation method
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Embodiment 1
Reclaim a method for the utilized material in production of chloroacetic acid tail gas, it is characterized in that, comprise the following steps:
(1) tail gas produced Mono Chloro Acetic Acid and produce is got, first reclaim through-15 DEG C of condensations and obtain low-boiling point material, and then obtaining low-boiling point material through-30 DEG C of condensations recovery, merging is reclaimed the low-boiling point materials such as Acetyl Chloride 98Min., chloroacetyl chloride and the acetic acid obtained and is continued transported to reactive system continuation reaction;
(2) step (1) condensed hydrogen chloride gas is got, being passed into volume tank adopts volumetric concentration to be 10% dilute hydrochloric acid washing absorption, make the Acetyl Chloride 98Min. in hydrogen chloride gas, chloroacetyl chloride, water in acetic acid and dilute hydrochloric acid reacts, be reduced into acetic acid and Mono Chloro Acetic Acid, when in the dilute hydrochloric acid in volume tank, moisture content reaches after below 1%, this washings continues reaction as raw material input response system; Washing tank continues to change dilute hydrochloric acid and remakes washings;
(3) get the hydrogen chloride gas after step (2) washing, absorb at clean absorption equipment internal recycle by purified water;
(4) remove solution heat in absorption process, prepare the refining hydrochloric acid of purity more than 99.98%.
Embodiment 2
Reclaim a method for the utilized material in production of chloroacetic acid tail gas, comprise the following steps:
(1) tail gas produced Mono Chloro Acetic Acid and produce is got, first reclaim through-15 DEG C of condensations and obtain low-boiling point material, and then obtaining low-boiling point material through-30 DEG C of condensations recovery, merging is reclaimed the low-boiling point materials such as Acetyl Chloride 98Min., chloroacetyl chloride and the acetic acid obtained and is continued transported to reactive system continuation reaction;
(2) step (1) condensed hydrogen chloride gas is got, being passed into volume tank adopts volumetric concentration to be 20% dilute hydrochloric acid washing absorption, make the Acetyl Chloride 98Min. in hydrogen chloride gas, chloroacetyl chloride, water in acetic acid and dilute hydrochloric acid reacts, be reduced into acetic acid and Mono Chloro Acetic Acid, when in the dilute hydrochloric acid in volume tank, moisture content reaches after below 1%, this washings continues reaction as raw material input response system; Washing tank continues to change dilute hydrochloric acid and remakes washings;
(3) get the hydrogen chloride gas after step (2) washing, absorb at clean absorption equipment internal recycle by purified water;
(4) remove solution heat in absorption process, prepare the refining hydrochloric acid of purity more than 99.99%.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. reclaim a method for the utilized material in production of chloroacetic acid tail gas, it is characterized in that, comprise the following steps:
(1) tail gas produced Mono Chloro Acetic Acid and produce is got, first reclaim through-10 ~-15 DEG C of condensations and obtain low-boiling point material, and then obtaining low-boiling point material through-20 ~-30 DEG C of condensations recovery, merging is reclaimed the low-boiling point material obtained and is continued transported to reactive system continuation reaction;
(2) step (1) condensed hydrogen chloride gas is got, be passed into volume tank and adopt dilute hydrochloric acid washing absorption, make the Acetyl Chloride 98Min. in hydrogen chloride gas, chloroacetyl chloride, water in acetic acid and dilute hydrochloric acid reacts, be reduced into acetic acid and Mono Chloro Acetic Acid, when in the dilute hydrochloric acid in volume tank, moisture content reaches after below 1%, this washings continues reaction as raw material input response system; Washing tank continues to change dilute hydrochloric acid and remakes washings;
(3) get the hydrogen chloride gas after step (2) washing, absorb at clean absorption equipment internal recycle by purified water;
(4) remove solution heat in absorption process, prepare the refining hydrochloric acid of purity more than 99.9%.
2. the method for the utilized material in recovery production of chloroacetic acid tail gas according to claim 1, it is characterized in that, step (1) gets the tail gas produced Mono Chloro Acetic Acid and produce, first reclaim through-15 DEG C of condensations and obtain low-boiling point material, and then obtaining low-boiling point material through-30 DEG C of condensations recovery, merging is reclaimed the low-boiling point material obtained and is continued transported to reactive system continuation reaction.
3. the method for the utilized material in recovery production of chloroacetic acid tail gas according to claim 1, it is characterized in that, the low-boiling point material described in step (1) is Acetyl Chloride 98Min., chloroacetyl chloride and acetic acid.
4. the method for the utilized material in recovery production of chloroacetic acid tail gas according to claim 1, is characterized in that, step (2) washing adopt dilute hydrochloric acid be volume dense be 10% ~ 30% hydrochloric acid.
5. the method for the utilized material in recovery production of chloroacetic acid tail gas according to claim 4, is characterized in that, removes solution heat in step (5) with less than 10 DEG C water coolants.
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| CN201510451831.5A CN105129734A (en) | 2015-07-28 | 2015-07-28 | Method for recovering available substances in chloroacetic acid production tail gas |
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| CN201510451831.5A CN105129734A (en) | 2015-07-28 | 2015-07-28 | Method for recovering available substances in chloroacetic acid production tail gas |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837175A (en) * | 2006-04-28 | 2006-09-27 | 石家庄东华金龙化工有限公司 | Improvement of preparation process for chloroacetic acid |
| CN101190396A (en) * | 2006-11-28 | 2008-06-04 | 张天德 | Chloroethanoic acid tail gas purifying and comprehensive utilization method |
| CN101219943A (en) * | 2007-01-08 | 2008-07-16 | 张天德 | Method for purifying and using chloroethanoic acid tail gas |
| CN102249189A (en) * | 2011-05-27 | 2011-11-23 | 许昌东方化工有限公司 | Method for recycling hydrochloric acid in chloroacetic acid production process |
| CN102816045A (en) * | 2012-09-05 | 2012-12-12 | 河北科技大学 | Method for synthesizing chloromethane by tail gas generated during chloroacetic acid production |
| CN104353345A (en) * | 2014-11-11 | 2015-02-18 | 许昌东方化工有限公司 | Tail gas treatment method in chloroacetic acid production process |
-
2015
- 2015-07-28 CN CN201510451831.5A patent/CN105129734A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837175A (en) * | 2006-04-28 | 2006-09-27 | 石家庄东华金龙化工有限公司 | Improvement of preparation process for chloroacetic acid |
| CN101190396A (en) * | 2006-11-28 | 2008-06-04 | 张天德 | Chloroethanoic acid tail gas purifying and comprehensive utilization method |
| CN101219943A (en) * | 2007-01-08 | 2008-07-16 | 张天德 | Method for purifying and using chloroethanoic acid tail gas |
| CN102249189A (en) * | 2011-05-27 | 2011-11-23 | 许昌东方化工有限公司 | Method for recycling hydrochloric acid in chloroacetic acid production process |
| CN102816045A (en) * | 2012-09-05 | 2012-12-12 | 河北科技大学 | Method for synthesizing chloromethane by tail gas generated during chloroacetic acid production |
| CN104353345A (en) * | 2014-11-11 | 2015-02-18 | 许昌东方化工有限公司 | Tail gas treatment method in chloroacetic acid production process |
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Application publication date: 20151209 |