CN102140055A - Purification method of chloridized liquid - Google Patents
Purification method of chloridized liquid Download PDFInfo
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- CN102140055A CN102140055A CN2010106171621A CN201010617162A CN102140055A CN 102140055 A CN102140055 A CN 102140055A CN 2010106171621 A CN2010106171621 A CN 2010106171621A CN 201010617162 A CN201010617162 A CN 201010617162A CN 102140055 A CN102140055 A CN 102140055A
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Abstract
The invention provides a purification method of a chloridized liquid. The purification method comprises three-stage washing steps, namely successively carrying out first-stage washing, second-stage washing and third-stage washing on the chloridized liquid. The purification method is characterized in that when the weight percents of hydrogen chloride and ferric trichloride in the three-stage washing water of the third-stage washing step reach 1%, feeding the three-stage washing water to the second-stage washing step, and synchronously supplementing clean water to the third-stage washing step; when the weight percents of hydrogen chloride and ferric trichloride in the second-stage washing water of the second-stage washing step reach 5%, feeding the second-stage washing water to the first-stage washing step; and when the weight percents of hydrogen chloride and ferric trichloride in the first-stage washing water of the first-stage washing step reach 10%, feeding the first-stage washing water to a crystallization kettle for concentrating and crystallizing the first-stage washing water, and removing hydrogen chloride so as to obtain solid ferric trichloride. A pipeline static mixer in which chlorination liquid and correspondingly washing water are mixed is arranged in each washing step. By using the method, the purification effect is good.
Description
Technical field
The present invention relates to the method for purification of the chlorated liquid in a kind of single benzene chloride production, to remove impurity such as hydrogenchloride in the chlorated liquid and iron trichloride.
Background technology
Purified petroleum benzin is by the effect of catalyzer (being generally iron trichloride), and by chlorinated with chlorine, it is acid that the chlorated liquid behind the chloride process is, and contain impurity such as hydrogenchloride and iron trichloride in chlorinator.Existing method of purification is that the acid chlorization liquid that contains impurity is once washed earlier, carry out an alkali cleaning again, in other words: add water in the acid chlorization liquid and mixing with it, wherein hydrogenchloride and iron trichloride are extracted in the wash water, and then diluted alkaline joined in the acid chlorization liquid after the washing, remove remaining hydrogenchloride and iron trichloride in the chlorated liquid, so that chlorated liquid is neutrality or slight alkalinity.
The shortcoming of existing method of purification is:
1, in water-washing step, the wash water and the chlorated liquid that add can not well mix (being that mixedness is not high), and the amount of water of appropriateness and enough mixedness are the key factors that guarantees chlorated liquid purification quality, cause to reduce well the content of iron trichloride and hydrogenchloride in the chlorated liquid, increased the alkali charge of follow-up alkali cleaning step, in addition, also may cause system's band acidity, then etching apparatus.
2, in the alkali cleaning step, iron trichloride and alkali reaction generate the ironic hydroxide flocks, when separation is thorough, this precipitation can be taken subsequent handling to, easily in reboiler import and export place's coking of distillation tower, causes reboiler to stop up, and then the increase steam consumption, unfavorable to system's operation;
3, the iron trichloride as catalyzer can not get recycle, causes the waste of resource, increases the enterprise operation cost.
Summary of the invention
The technical problem to be solved in the present invention provides the method for purification of the good chlorated liquid of a kind of refining effect.
For solving the problems of the technologies described above, the invention provides a kind of method of purification of chlorated liquid, comprise that first step washing, the second stage that chlorated liquid is carried out are successively washed, three grades of water-washing steps of third stage washing.
For can concise description for the purpose of the problem, below the method for purification of chlorated liquid of the present invention be all abbreviated as present method.
Present method has been saved the alkali cleaning step in the background technology, exempted the ironic hydroxide flocks damage system device that generates in the alkali cleaning step, reduced the energy consumption material consumption, production cost reaches the pressure to subsequent handling equipment, reduced pollution to environment, and only need through three grades of water-washing steps, centrifugation by water, realized the thorough mixing of chlorated liquid and water, can obtain to satisfy the chlorated liquid of purity requirement with impurity such as hydrogenchloride contained in the chlorated liquid and iron trichloride are most of removes (be hydrogenchloride contained in the chlorated liquid can enter in the wash water of corresponding stage with iron trichloride and well separated).
As the optimization of present method, when the weight percent concentration of hydrogenchloride in three grades of wash waters of third stage water-washing step and iron trichloride reaches 1%, three grades of wash waters are sent into second stage water-washing step, replenish water purification to third stage water-washing step synchronously; When the weight percent concentration of hydrogenchloride in the secondary wash water of second stage water-washing step and iron trichloride reaches 5%, the secondary wash water is sent into first step water-washing step; When the weight percent concentration of hydrogenchloride in the one-level wash water of first step water-washing step and iron trichloride reaches 10%, the one-level wash water is sent into crystallization kettle it is carried out condensing crystal, remove behind the hydrogenchloride the solid phase iron trichloride.
Present method adds to back one-level wash water and continues to apply mechanically in the previous stage water-washing step, like this, make wash water in system, obtain recycled, and the solid phase iron trichloride can carry it into chlorinator by benzene feedstock, thereby realize of the recycle of solid phase iron trichloride, save related resource, further reduce production costs as catalyzer.
As the further optimization of present method, be equipped with in every grade of water-washing step and make chlorated liquid and corresponding stage wash water carry out the blended pipeline static mixer.
The setting of pipeline static mixer, make chlorated liquid and corresponding stage wash water thorough mixing, improved mixedness, strengthened the washing effect of chlorated liquid, separate impurities efficient is higher.
According to measuring and calculating, adopt present method, produce monochlor(in)ate benzene per ton, can reduce caustic soda consumption 3Kg, iron hoop consumption 1Kg, calculate by the monochlor(in)ate benzene device of producing 150000 tons per year, can save production cost every year thus about 3,500,000 yuan.
Description of drawings
Fig. 1 is the technological process block-diagram of present method.
Embodiment
Below in conjunction with accompanying drawing embodiments of the present invention are specifically described:
Referring to Fig. 1: present method comprises three grades of water-washing steps of first step washing that chlorated liquid is carried out successively, second stage washing, third stage washing, and three steps are corresponding first step washing equipment, second stage washing equipment, third stage washing equipment respectively.
First step washing equipment comprises one-level pipeline static mixer, one-level washing pump, one-level washing separator, one-level wash water circulation groove, the one-level wash water recycle pump that joins by corresponding pipeline and valve (not shown its piece number in the accompanying drawing), described pipeline is pipeline 12, pipeline 13, pipeline 14, pipeline 15, pipeline 16, in addition, pipeline 11 joins with chlorinator and one-level pipeline static mixer respectively, and the outlet end of one-level wash water recycle pump also joins with crystallization kettle by pipeline 17 and valve (not shown its piece number in the accompanying drawing).The one-level pipeline static mixer is arranged on before the one-level washing pump.
Second stage washing equipment comprises the secondary pipeline static mixer that joins by corresponding pipeline and valve (not shown its piece number in the accompanying drawing), secondary washing pump, secondary washing separator, secondary wash water circulation groove, secondary wash water recycle pump, described pipeline is a pipeline 22, pipeline 23, pipeline 24, pipeline 25, pipeline 26, in addition, pipeline 21 joins with the last outlet end of one-level washing separator and the liquid feeding end of secondary pipeline static mixer respectively, and the outlet end of secondary wash water recycle pump also joins by the last liquid feeding end of pipeline 27 and valve (not shown its piece number in the accompanying drawing) and one-level wash water circulation groove.The secondary pipeline static mixer is arranged on before the secondary washing pump.
Third stage washing equipment comprises the triode road static mixer that joins by corresponding pipeline and valve (not shown its piece number in the accompanying drawing), three grades of washing pumps, three grades of washing separators, three grades of wash water circulation grooves, three grades of wash water recycle pumps, described pipeline is a pipeline 32, pipeline 33, pipeline 34, pipeline 35, pipeline 36, in addition, pipeline 31 joins with the last outlet end of secondary washing separator and the liquid feeding end of triode road static mixer respectively, the outlet end of three grades of wash water recycle pumps also joins by the last liquid feeding end of pipeline 37 and valve (not shown its piece number in the accompanying drawing) and secondary wash water circulation groove, the last outlet end of three grades of washing separators also joins by pipeline 38 and chlorated liquid moisture eliminator, and the last liquid feeding end of three grades of wash water circulation grooves also joins by pipeline 39 and tap water water source.Triode road static mixer is arranged on before three grades of washing pumps.
Like this, be equipped with in every grade of water-washing step and make chlorated liquid and corresponding stage wash water carry out the blended pipeline static mixer.
For first step water-washing step: the chlorated liquid from chlorinator passes through pipeline 11, one-level wash water from one-level wash water recycle pump enters in the one-level pipeline static mixer jointly by pipeline 16, make described chlorated liquid and one-level wash water thorough mixing, mixed solution is through pipeline 12 then, one-level washing pump, pipeline 13 enters one-level washing separator and (hydrogenchloride in the chlorated liquid and iron trichloride is extracted in the one-level wash water, make the one-level wash water contain acidity), enter the liquid feeding end (promptly entering second stage water-washing step) of secondary pipeline static mixer through pipeline 21 from the effusive one-level chlorated liquid of last outlet end of one-level washing separator, and the following outlet end that the one-level wash water is washed separator from one-level enters one-level wash water circulation groove automatically by pipeline 14, described one-level wash water is by pipeline 15, one-level wash water recycle pump, pipeline 16 enters in the one-level pipeline static mixer, and and from the chlorated liquid of chlorinator thorough mixing once more, like this, described one-level wash water carries out internal recycle in a manner described again and again in first step washing equipment, when the weight percent concentration of hydrogenchloride in the one-level wash water and iron trichloride reaches 10%, by one-level wash water recycle pump, pipeline 17 is sent the one-level wash water into crystallization kettle it is carried out condensing crystal (being that the one-level wash water carries out outer circulation), remove behind the hydrogenchloride the solid phase iron trichloride.
For the water-washing step of the second stage: the one-level chlorated liquid from one-level washing separator passes through pipeline 21, secondary wash water from secondary wash water recycle pump enters in the secondary pipeline static mixer jointly by pipeline 26, make described chlorated liquid and secondary wash water thorough mixing, mixed solution is through pipeline 22 then, secondary washing pump, pipeline 23 enters secondary washing separator and (hydrogenchloride in the chlorated liquid and iron trichloride is extracted in the secondary wash water, make the secondary wash water contain acidity), enter the liquid feeding end (promptly entering third stage water-washing step) of triode road static mixer through pipeline 31 from the effusive secondary chlorination liquid of last outlet end of secondary washing separator, and the following outlet end that the secondary wash water is washed separator from secondary enters secondary wash water circulation groove automatically by pipeline 24, described secondary wash water is by pipeline 25, secondary wash water recycle pump, pipeline 26 enters in the secondary pipeline static mixer, and and from the one-level chlorated liquid of one-level washing separator thorough mixing once more, like this, described secondary wash water carries out internal recycle in a manner described again and again in the washing equipment of the second stage, when the weight percent concentration of hydrogenchloride in the secondary wash water and iron trichloride reaches 5%, by secondary wash water recycle pump, pipeline 27 is sent the secondary wash water into the last liquid feeding end of one-level wash water circulation groove, and described secondary wash water obtains recycling (being that the secondary wash water carries out outer circulation) in first step water-washing step.
For third stage water-washing step: the secondary chlorination liquid from secondary washing separator passes through pipeline 31, three grades of wash waters from three grades of wash water recycle pumps enter in the triode road static mixer jointly by pipeline 36, make described chlorated liquid and three grades of wash water thorough mixing, mixed solution is through pipeline 32 then, three grades of washing pumps, pipeline 33 enters three grades of washing separators and (hydrogenchloride in the chlorated liquid and iron trichloride is extracted in three grades of wash waters, make three grades of wash waters contain acidity), three grades of wash waters enter three grades of wash water circulation grooves from three grades of following outlet ends of washing separators automatically by pipeline 34, described three grades of wash waters are by pipeline 35, three grades of wash water recycle pumps, pipeline 36 enters in the triode road static mixer, and and from the secondary chlorination liquid of secondary washing separator thorough mixing once more, like this, described three grades of wash waters carry out internal recycle in a manner described again and again in third stage washing equipment, when the weight percent concentration of hydrogenchloride in three grades of wash waters and iron trichloride reaches 1%, by three grades of wash water recycle pumps, the last liquid feeding end of secondary wash water circulation groove sent into three grades of wash waters by pipeline 37, described three grades of wash waters obtain recycling (promptly three grades of wash waters carry out outer circulation) in the water-washing step of the second stage, meanwhile, in three grades of wash water circulation grooves, replenish water purification by pipeline 39, in addition, deliver to the chlorated liquid moisture eliminator from the effusive three grades of chlorated liquids of last outlet end of three grades of washing separators by pipeline 38 and separate drying.
In sum, the flow direction of chlorated liquid is followed successively by: first step washing, second stage washing, third stage washing; And the flow direction of wash water is followed successively by: third stage washing, second stage washing, first step washing.
Above-described only is one embodiment of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the principle of the invention, can also make conspicuous some conversion or alternative and remodeling, these also should be considered as belonging to protection scope of the present invention.
Claims (3)
1. the method for purification of chlorated liquid comprises that first step washing, the second stage that chlorated liquid is carried out are successively washed, three grades of water-washing steps of third stage washing.
2. the method for purification of chlorated liquid according to claim 1, it is characterized in that: when the weight percent concentration of hydrogenchloride in three grades of wash waters of third stage water-washing step and iron trichloride reaches 1%, three grades of wash waters are sent into second stage water-washing step, replenish water purification to third stage water-washing step synchronously; When the weight percent concentration of hydrogenchloride in the secondary wash water of second stage water-washing step and iron trichloride reaches 5%, the secondary wash water is sent into first step water-washing step; When the weight percent concentration of hydrogenchloride in the one-level wash water of first step water-washing step and iron trichloride reaches 10%, the one-level wash water is sent into crystallization kettle it is carried out condensing crystal, remove behind the hydrogenchloride the solid phase iron trichloride.
3. the method for purification of chlorated liquid according to claim 1 and 2 is characterized in that: be equipped with in every grade of water-washing step and make chlorated liquid and corresponding stage wash water carry out the blended pipeline static mixer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201010617162.1A CN102140055B (en) | 2010-12-29 | 2010-12-29 | Purification method of chloridized liquid |
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| CN201010617162.1A CN102140055B (en) | 2010-12-29 | 2010-12-29 | Purification method of chloridized liquid |
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| CN102140055A true CN102140055A (en) | 2011-08-03 |
| CN102140055B CN102140055B (en) | 2014-03-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584523A (en) * | 2012-01-31 | 2012-07-18 | 杨瑞良 | Semifinished chlorinated solution water washing and alkali washing device used during chlorobenzene production and water washing and alkali washing method |
| CN103819306A (en) * | 2014-02-02 | 2014-05-28 | 安徽八一化工股份有限公司 | Technology for removing ferric trichloride from chlorination liquid generated in chlorobenzene production |
| CN108721942A (en) * | 2018-06-04 | 2018-11-02 | 甘肃泓旭化工科技有限责任公司 | A kind of continuous flow upstream extraction of liquid phase mixture washes reaction process and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102584523A (en) * | 2012-01-31 | 2012-07-18 | 杨瑞良 | Semifinished chlorinated solution water washing and alkali washing device used during chlorobenzene production and water washing and alkali washing method |
| CN102584523B (en) * | 2012-01-31 | 2014-03-26 | 杨瑞良 | Semifinished chlorinated solution water washing and alkali washing device used during chlorobenzene production and water washing and alkali washing method |
| CN103819306A (en) * | 2014-02-02 | 2014-05-28 | 安徽八一化工股份有限公司 | Technology for removing ferric trichloride from chlorination liquid generated in chlorobenzene production |
| CN103819306B (en) * | 2014-02-02 | 2015-10-28 | 安徽八一化工股份有限公司 | The technique of iron trichloride is removed in the chlorated liquid that production Benzene Chloride produces |
| CN108721942A (en) * | 2018-06-04 | 2018-11-02 | 甘肃泓旭化工科技有限责任公司 | A kind of continuous flow upstream extraction of liquid phase mixture washes reaction process and application |
| CN108721942B (en) * | 2018-06-04 | 2024-01-26 | 甘肃泓旭化工科技有限责任公司 | Continuous countercurrent reaction process of liquid phase mixture and application |
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| CN102140055B (en) | 2014-03-12 |
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