CN105294420A - Stearoyl chloride waste material treating method - Google Patents
Stearoyl chloride waste material treating method Download PDFInfo
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- CN105294420A CN105294420A CN201510692505.3A CN201510692505A CN105294420A CN 105294420 A CN105294420 A CN 105294420A CN 201510692505 A CN201510692505 A CN 201510692505A CN 105294420 A CN105294420 A CN 105294420A
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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 provides a stearoyl chloride waste material treating method. The method comprises the following steps that firstly, coarse stearoyl chloride is heated; secondly, an activated carbon adsorbent is added in the coarse stearoyl chloride; thirdly, primary cooling is performed on liquid obtained after activated carbon adsorption; fourthly, high-temperature evaporation is performed on residues obtained through filtration; fifthly, gas generated through evaporation is collected, and then secondary cooling is performed on the gas; sixthly, the materials processed through secondary cooling are sent into a dryer and a sprayer to be dried; lastly, the dried materials are introduced into a concentrator to be concentrated, collecting is performed, and then further treating is performed. According to the stearoyl chloride waste material treating method, by adopting the production technology, tar substances in the coarse stearoyl chloride can be thoroughly separated; meanwhile, a side reaction can be prevented from being further generated to influence the purity of stearoyl chloride when the coarse stearoyl chloride is separated again at the certain temperature and time under the certain pressure.
Description
Technical field
The present invention relates to plastics fine chemistry industry production field, be specifically related to a kind of method for treatment of waste material of stearic acid chloride.
Background technology
Stearyl chloride (Stearoylacidchloride; have another name called stearoyl chlorine) be a kind of pesticide intermediate; also be the raw materials for production of the rare ketone dimer (AKD) of papermaking neutral sizing agent--alkyl; by industrial stearic acid under the catalysis of catalyzer dimethyl formamide (DMF), the acylate generated with phosgene reaction.Its reaction is mainly divided into two stages:
1, the catalyst activation stage
Phosgene and dimethyl formamide react and generate active group (1), and active group (1) is very unstable, releases the CO of a part very soon
2, and generate active group (2);
2, active group (2) and stearic acid react and generate stearyl chloride, and regenerate dimethyl formamide, release the HCl of a part simultaneously;
Thick stearyl chloride decolouring at present generally adopts active carbon absorption technology, a certain amount of active carbon powder is added in thick and stiff acyl chlorine products, be uniformly mixed adsorption bleaching, and then adopt pressure filter to be separated the gac deviating to be adsorbed with tar, obtain yellowish stearyl chloride product.The acyl chlorides colourity that the method obtains is higher, poor product quality, and personnel labor intensity is large, and operating environment is poor.Add active carbon powder amount in treating processes large, production cost is high, fixed-end forces difficulty.
Summary of the invention
For above problems of the prior art, the invention provides a kind of method for treatment of waste material of stearic acid chloride, reduce the cost of process, improve the effect of process.
The present invention is achieved by the following technical solutions:
A method for treatment of waste material for stearic acid chloride, its step is as follows:
1) thick stearyl chloride is heated to 75-120 DEG C stand-by;
2) be heated to add acticarbon in step 1 to the thick stearyl chloride of 75-120 DEG C;
3) liquid after the charcoal absorption in step 2 is once cooled, and temperature is cooled to 75-85 DEG C, rear filtration;
4) residue after filtration in step 3 is carried out high temperature evaporation, and temperature during evaporation is 155-165 DEG C, the time is 30-45 minute, and wherein pressure is 0.15MPa-0.45MPa;
5) gas after evaporation in step 4 is collected, and by gas cooling twice, and cooling temperature is to 75-85 DEG C;
6) carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in step 5;
7) dried for step 6 material is passed in thickener concentrates, collect and process further again.
Further, a kind of method for treatment of waste material of stearic acid chloride, its step is as follows:
1) thick stearyl chloride is heated to 75-120 DEG C stand-by;
2) be heated to add acticarbon in step 1 to the thick stearyl chloride of 75-120 DEG C;
3) liquid after the charcoal absorption in step 2 is once cooled, and temperature is cooled to 75-85 DEG C, rear filtration;
4) residue after filtration in step 3 is carried out high temperature evaporation, and temperature during evaporation is 155-165 DEG C, the time is 30-45 minute, and wherein pressure is 0.15MPa-0.45MPa;
5) gas after evaporation in step 4 is collected, and by gas cooling twice, and cooling temperature is to 75-85 DEG C;
6) carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in step 5;
7) dried for step 6 material is passed in thickener concentrates, collect and process further again.
Beneficial effect of the present invention is: the present invention adopts above-mentioned production technique, the contact area of reactant can be increased, reduce the reaction times, simultaneous temperature controls very important, increasing of by product can be avoided, therefore just improve reaction efficiency, cost reduces, decrease the waste of phosgene, decrease the time of material post-processed such as rectifying and off gas treatment, wherein, save phosgene 10-15%, the content of thick polyester acyl chlorides is increased to 79-88%, and cost savings 23-30%, the time saves 2-3.5 hour.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
First thick stearyl chloride is heated to 105 DEG C stand-by, can be easy to the later stage carries out charcoal absorption impurity;
Secondly to the thick stearyl chloride of 105 DEG C, acticarbon is added to aforementioned being heated to, can by the impurity of said temperature, as tar-like substance adsorbs, therefore and simultaneously heat-up time time is 11s, avoid thick and stiff matter acyl chlorides to be at high temperature easier to generate more tar-like substance like this, therefore the tar-like substance in thick and stiff matter acyl chlorides can be separated by gac;
Again the liquid after aforesaid charcoal absorption is once cooled, and temperature is cooled to 80 DEG C, rear filtration, rapidly after cooling, the gac adsorbing tar-like substance can be carried out filtering separation;
Thirdly the residue after foregoing filtration is carried out high temperature evaporation, and temperature during evaporation is 158 DEG C, the time is 40 minutes, and wherein pressure is 0.35MPa, wherein tar-like substance can be catalyzed into steam and Activated carbon separation, and this gac can recycling;
Again the gas after aforementioned middle evaporation is collected, and by gas cooling twice, and cooling temperature to 80 DEG C, tar-like substance can be cooled to liquid substance, convenient that tar-like substance is dry further;
Carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in aforementioned again, be easy to deposit after tar-like substance is carried out drying;
Finally aforementioned dried material is passed in thickener and concentrates, collect and process further again, be condensed into the material being easy to deposit, also facilitate the later stage to recycle simultaneously.
Therefore above-mentioned production technique is adopted, tar-like substance in thick and stiff matter acyl chlorides thoroughly can be separated, and have employed certain temperature and time, with under certain pressure, when thick and stiff matter acyl chlorides can be avoided to be separated again, further produce side reaction thus affect the purity of hard acyl chlorides, therefore have employed gac and thickener with the use of, gac can be recycled and reused simultaneously, the waste of raw material can be avoided, reduce production cost.
Embodiment 2
First thick stearyl chloride is heated to 75 DEG C stand-by, can be easy to the later stage carries out charcoal absorption impurity;
Secondly to the thick stearyl chloride of 75 DEG C, acticarbon is added to aforementioned being heated to, can by the impurity of said temperature, as tar-like substance adsorbs, therefore and simultaneously heat-up time time is 20s, avoid thick and stiff matter acyl chlorides to be at high temperature easier to generate more tar-like substance like this, therefore the tar-like substance in thick and stiff matter acyl chlorides can be separated by gac;
Again the liquid after aforesaid charcoal absorption is once cooled, and temperature is cooled to 75 DEG C, rear filtration, rapidly after cooling, the gac adsorbing tar-like substance can be carried out filtering separation;
Thirdly the residue after foregoing filtration is carried out high temperature evaporation, and temperature during evaporation is 155 DEG C, the time is 45 minutes, and wherein pressure is 0.15MPa, wherein tar-like substance can be catalyzed into steam and Activated carbon separation, and this gac can recycling;
Again the gas after aforementioned middle evaporation is collected, and by gas cooling twice, and cooling temperature to 75 DEG C, tar-like substance can be cooled to liquid substance, convenient that tar-like substance is dry further;
Carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in aforementioned again, be easy to deposit after tar-like substance is carried out drying;
Finally aforementioned dried material is passed in thickener and concentrates, collect and process further again, be condensed into the material being easy to deposit, also facilitate the later stage to recycle simultaneously.
Therefore above-mentioned production technique is adopted, tar-like substance in thick and stiff matter acyl chlorides thoroughly can be separated, and have employed certain temperature and time, with under certain pressure, when thick and stiff matter acyl chlorides can be avoided to be separated again, further produce side reaction thus affect the purity of hard acyl chlorides, therefore have employed gac and thickener with the use of, gac can be recycled and reused simultaneously, the waste of raw material can be avoided, reduce production cost.
Embodiment 3
First thick stearyl chloride is heated to 85 DEG C stand-by, can be easy to the later stage carries out charcoal absorption impurity;
Secondly to the thick stearyl chloride of 85 DEG C, acticarbon is added to aforementioned being heated to, can by the impurity of said temperature, as tar-like substance adsorbs, therefore and simultaneously heat-up time time is 16s, avoid thick and stiff matter acyl chlorides to be at high temperature easier to generate more tar-like substance like this, therefore the tar-like substance in thick and stiff matter acyl chlorides can be separated by gac;
Again the liquid after aforesaid charcoal absorption is once cooled, and temperature is cooled to 73 DEG C, rear filtration, rapidly after cooling, the gac adsorbing tar-like substance can be carried out filtering separation;
Thirdly the residue after foregoing filtration is carried out high temperature evaporation, and temperature during evaporation is 165 DEG C, the time is 30 minutes, and wherein pressure is 0.45MPa, wherein tar-like substance can be catalyzed into steam and Activated carbon separation, and this gac can recycling;
Again the gas after aforementioned middle evaporation is collected, and by gas cooling twice, and cooling temperature to 73 DEG C, tar-like substance can be cooled to liquid substance, convenient that tar-like substance is dry further;
Carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in aforementioned again, be easy to deposit after tar-like substance is carried out drying;
Finally aforementioned dried material is passed in thickener and concentrates, collect and process further again, be condensed into the material being easy to deposit, also facilitate the later stage to recycle simultaneously.
Therefore above-mentioned production technique is adopted, tar-like substance in thick and stiff matter acyl chlorides thoroughly can be separated, and have employed certain temperature and time, with under certain pressure, when thick and stiff matter acyl chlorides can be avoided to be separated again, further produce side reaction thus affect the purity of hard acyl chlorides, therefore have employed gac and thickener with the use of, gac can be recycled and reused simultaneously, the waste of raw material can be avoided, reduce production cost.
Embodiment 4
First thick stearyl chloride is heated to 95 DEG C stand-by, can be easy to the later stage carries out charcoal absorption impurity;
Secondly to the thick stearyl chloride of 95 DEG C, acticarbon is added to aforementioned being heated to, can by the impurity of said temperature, as tar-like substance adsorbs, therefore and simultaneously heat-up time time is 13s, avoid thick and stiff matter acyl chlorides to be at high temperature easier to generate more tar-like substance like this, therefore the tar-like substance in thick and stiff matter acyl chlorides can be separated by gac;
Again the liquid after aforesaid charcoal absorption is once cooled, and temperature is cooled to 83 DEG C, rear filtration, rapidly after cooling, the gac adsorbing tar-like substance can be carried out filtering separation;
Thirdly the residue after foregoing filtration is carried out high temperature evaporation, and temperature during evaporation is 160 DEG C, the time is 35 minutes, and wherein pressure is 0.25MPa, wherein tar-like substance can be catalyzed into steam and Activated carbon separation, and this gac can recycling;
Again the gas after aforementioned middle evaporation is collected, and by gas cooling twice, and cooling temperature to 83 DEG C, tar-like substance can be cooled to liquid substance, convenient that tar-like substance is dry further;
Carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in aforementioned again, be easy to deposit after tar-like substance is carried out drying;
Finally aforementioned dried material is passed in thickener and concentrates, collect and process further again, be condensed into the material being easy to deposit, also facilitate the later stage to recycle simultaneously.
Therefore above-mentioned production technique is adopted, tar-like substance in thick and stiff matter acyl chlorides thoroughly can be separated, and have employed certain temperature and time, with under certain pressure, when thick and stiff matter acyl chlorides can be avoided to be separated again, further produce side reaction thus affect the purity of hard acyl chlorides, therefore have employed gac and thickener with the use of, gac can be recycled and reused simultaneously, the waste of raw material can be avoided, reduce production cost.
Embodiment 5
First thick stearyl chloride is heated to 120 DEG C stand-by, can be easy to the later stage carries out charcoal absorption impurity;
Secondly to the thick stearyl chloride of 120 DEG C, acticarbon is added to aforementioned being heated to, can by the impurity of said temperature, as tar-like substance adsorbs, therefore and simultaneously heat-up time time is 10s, avoid thick and stiff matter acyl chlorides to be at high temperature easier to generate more tar-like substance like this, therefore the tar-like substance in thick and stiff matter acyl chlorides can be separated by gac;
Again the liquid after aforesaid charcoal absorption is once cooled, and temperature is cooled to 85 DEG C, rear filtration, rapidly after cooling, the gac adsorbing tar-like substance can be carried out filtering separation;
Thirdly the residue after foregoing filtration is carried out high temperature evaporation, and the temperature 163 DEG C during evaporation, the time is 38 minutes, and wherein pressure is 0.40MPa, wherein tar-like substance can be catalyzed into steam and Activated carbon separation, and this gac can recycling;
Again the gas after aforementioned middle evaporation is collected, and by gas cooling twice, and cooling temperature to 85 DEG C, tar-like substance can be cooled to liquid substance, convenient that tar-like substance is dry further;
Carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in aforementioned again, be easy to deposit after tar-like substance is carried out drying;
Finally aforementioned dried material is passed in thickener and concentrates, collect and process further again, be condensed into the material being easy to deposit, also facilitate the later stage to recycle simultaneously.
Therefore above-mentioned production technique is adopted, tar-like substance in thick and stiff matter acyl chlorides thoroughly can be separated, and have employed certain temperature and time, with under certain pressure, when thick and stiff matter acyl chlorides can be avoided to be separated again, further produce side reaction thus affect the purity of hard acyl chlorides, therefore have employed gac and thickener with the use of, gac can be recycled and reused simultaneously, the waste of raw material can be avoided, reduce production cost.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. a method for treatment of waste material for stearic acid chloride, is characterized in that: its step is as follows:
1) thick stearyl chloride is heated to 75-120 DEG C stand-by;
2) be heated to add acticarbon in step 1 to the thick stearyl chloride of 75-120 DEG C;
3) liquid after the charcoal absorption in step 2 is once cooled, and temperature is cooled to 75-85 DEG C, rear filtration;
4) residue after filtration in step 3 is carried out high temperature evaporation, and temperature during evaporation is 155-165 DEG C, the time is 30-45 minute, and wherein pressure is 0.15MPa-0.45MPa;
5) gas after evaporation in step 4 is collected, and by gas cooling twice, and cooling temperature is to 75-85 DEG C;
6) carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in step 5;
7) dried for step 6 material is passed in thickener concentrates, collect and process further again.
2. the method for treatment of waste material of a kind of stearic acid chloride according to claim 1, is characterized in that: its step is as follows:
1) thick stearyl chloride is heated to 75-120 DEG C stand-by;
2) be heated to add acticarbon in step 1 to the thick stearyl chloride of 75-120 DEG C;
3) liquid after the charcoal absorption in step 2 is once cooled, and temperature is cooled to 75-85 DEG C, rear filtration;
4) residue after filtration in step 3 is carried out high temperature evaporation, and temperature during evaporation is 155-165 DEG C, the time is 30-45 minute, and wherein pressure is 0.15MPa-0.45MPa;
5) gas after evaporation in step 4 is collected, and by gas cooling twice, and cooling temperature is to 75-85 DEG C;
6) carry out moisture eliminator atomizer carry out drying by carrying out the material after cooling twice in step 5;
7) dried for step 6 material is passed in thickener concentrates, collect and process further again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510692505.3A CN105294420B (en) | 2015-10-20 | 2015-10-20 | Stearoyl chloride waste material treating method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510692505.3A CN105294420B (en) | 2015-10-20 | 2015-10-20 | Stearoyl chloride waste material treating method |
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| CN105294420B CN105294420B (en) | 2017-03-22 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01211547A (en) * | 1988-02-18 | 1989-08-24 | Nippon Oil & Fats Co Ltd | Purification of acyl halide |
| US6770783B1 (en) * | 1999-09-13 | 2004-08-03 | Basf Aktiengesellschaft | Method for producing acid chlorides |
| CN104592003A (en) * | 2014-12-29 | 2015-05-06 | 甘肃银光聚银化工有限公司 | Decoloring method of crude stearyl chloride |
-
2015
- 2015-10-20 CN CN201510692505.3A patent/CN105294420B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01211547A (en) * | 1988-02-18 | 1989-08-24 | Nippon Oil & Fats Co Ltd | Purification of acyl halide |
| US6770783B1 (en) * | 1999-09-13 | 2004-08-03 | Basf Aktiengesellschaft | Method for producing acid chlorides |
| CN104592003A (en) * | 2014-12-29 | 2015-05-06 | 甘肃银光聚银化工有限公司 | Decoloring method of crude stearyl chloride |
Non-Patent Citations (2)
| Title |
|---|
| 李文明等: "活性炭再生方法的分析和比较", 《广州化工》 * |
| 翁元声: "活性炭再生及新技术研究", 《给水排水》 * |
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