CN102140055B - Purification method of chloridized liquid - Google Patents
Purification method of chloridized liquid Download PDFInfo
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- CN102140055B CN102140055B CN201010617162.1A CN201010617162A CN102140055B CN 102140055 B CN102140055 B CN 102140055B CN 201010617162 A CN201010617162 A CN 201010617162A CN 102140055 B CN102140055 B CN 102140055B
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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 the impurity such as hydrogenchloride in chlorated liquid and iron trichloride.
Background technology
Purified petroleum benzin is by the effect of catalyzer (being generally iron trichloride), and in chlorinator, by chlorinated with chlorine, it is acid that the chlorated liquid after chloride process is, and contain the impurity such as hydrogenchloride and iron trichloride.Existing method of purification is that the acid chlorization liquid that contains impurity is first once washed, carry out again an alkali cleaning, in other words: water is added in acid chlorization liquid and with it and mixed, hydrogenchloride wherein and iron trichloride are extracted in wash water, and then diluted alkaline is joined in the acid chlorization liquid after washing, remove remaining hydrogenchloride and iron trichloride in 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 adding and chlorated liquid 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 reducing well the content of iron trichloride and hydrogenchloride in chlorated liquid, increased the alkali charge of follow-up alkali cleaning step, in addition, also may cause system band acid, then etching apparatus.
2, in alkali cleaning step, iron trichloride and alkali reaction generate ironic hydroxide flocks, when separation is not 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 increase steam consumption, unfavorable to system operation;
3, the iron trichloride as catalyzer can not get recycle, causes the waste of resource, increases enterprise operation cost.
Summary of the invention
The technical problem to be solved in the present invention is to provide the method for purification of the chlorated liquid that a kind of refining effect is good.
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 problem, below to the method for purification of chlorated liquid of the present invention all referred to as present method.
Present method has been saved the alkali cleaning step in background technology, exempted the ironic hydroxide flocks damage system device generating in alkali cleaning step, reduced energy and material consumption, production cost and the pressure to subsequent handling equipment, reduced the pollution to environment, and only need be through three grades of water-washing steps, by the centrifugation of water, realized the abundant mixing of chlorated liquid and water, can be by the impurity such as hydrogenchloride contained in chlorated liquid and iron trichloride be most of removes (be hydrogenchloride contained in chlorated liquid can enter in the wash water of corresponding stage with iron trichloride and obtain good separated), acquisition meets the chlorated liquid of purity requirement.
As the optimization of present method, when the hydrogenchloride in three grades of wash waters of third stage water-washing step and the weight percent concentration of iron trichloride reach 1%, three grades of wash waters are sent into second stage water-washing step, synchronously to third stage water-washing step, supplement water purification; When the hydrogenchloride in the secondary wash water of second stage water-washing step and the weight percent concentration of iron trichloride reach 5%, secondary wash water is sent into first step water-washing step; When the hydrogenchloride in the one-level wash water of first step water-washing step and the weight percent concentration of iron trichloride reach 10%, one-level wash water is sent into crystallization kettle it is carried out to condensing crystal, remove after hydrogenchloride to obtain solid phase iron trichloride.
Present method adds to rear one-level wash water in previous stage water-washing step and continues to apply mechanically, like this, make wash water in system, obtain recycled, and solid phase iron trichloride can carry it into chlorinator by benzene feedstock, thereby realize solid phase iron trichloride as the recycle of catalyzer, save related resource, further reduce production costs.
As the further optimization of present method, in every grade of water-washing step, be equipped with the pipeline static mixer that chlorated liquid and corresponding stage wash water are mixed.
The setting of pipeline static mixer, makes chlorated liquid and corresponding stage wash water fully mix, improve mixedness, has strengthened the washing effect of chlorated liquid, and the separation efficiency of impurity is higher.
According to measuring and calculating, adopt present method, produce chlorobenzene per ton, can reduce caustic soda consumption 3Kg, iron hoop consumption 1Kg, by the chlorobenzene device of producing 150000 tons per year, calculate, can save production cost every year thus approximately 3,500,000 yuan.
Accompanying drawing explanation
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 joining by corresponding pipeline and valve (attached not shown its piece number), described pipeline is pipeline 12, pipeline 13, pipeline 14, pipeline 15, pipeline 16, separately, 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 (attached not shown its piece number).Before one-level pipeline static mixer is arranged on one-level washing pump.
Second stage washing equipment comprises the secondary pipeline static mixer joining by corresponding pipeline and valve (attached not shown its piece number), secondary washing pump, secondary washing separator, secondary wash water circulation groove, secondary wash water recycle pump, described pipeline is pipeline 22, pipeline 23, pipeline 24, pipeline 25, pipeline 26, separately, pipeline 21 joins with the one-level washing upper outlet end of separator and the liquid feeding end of secondary pipeline static mixer respectively, the outlet end of secondary wash water recycle pump also joins with the upper liquid feeding end of one-level wash water circulation groove by pipeline 27 and valve (attached not shown its piece number).Before secondary pipeline static mixer is arranged on secondary washing pump.
Third stage washing equipment comprises the triode road static mixer joining by corresponding pipeline and valve (attached not shown its piece number), 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 pipeline 32, pipeline 33, pipeline 34, pipeline 35, pipeline 36, separately, pipeline 31 joins with the secondary washing upper outlet end of 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 with the upper liquid feeding end of secondary wash water circulation groove by pipeline 37 and valve (attached not shown its piece number), the upper outlet end of three grades of washing separators also joins by pipeline 38 and chlorated liquid moisture eliminator, the upper liquid feeding end of three grades of wash water circulation grooves also joins by pipeline 39 and tap water water source.Before triode road static mixer is arranged on three grades of washing pumps.
Like this, in every grade of water-washing step, be equipped with the pipeline static mixer that chlorated liquid and corresponding stage wash water are mixed.
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 one-level pipeline static mixer jointly by pipeline 16, described chlorated liquid is fully mixed with one-level wash water, then mixed solution is through pipeline 12, one-level washing pump, pipeline 13 enters one-level washing separator and (hydrogenchloride in chlorated liquid and iron trichloride is extracted in one-level wash water, make one-level wash water contain acidity), the one-level chlorated liquid that outlet end flows out from one-level washing separator enters the liquid feeding end (entering second stage water-washing step) of secondary pipeline static mixer through pipeline 21, and one-level wash water outlet end from one-level washing separator 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 one-level pipeline static mixer, and and from the chlorated liquid of chlorinator, again fully mix, like this, described one-level wash water carries out again and again in a manner described internal recycle in first step washing equipment, when the hydrogenchloride in one-level wash water and the weight percent concentration of iron trichloride reach 10%, by one-level wash water recycle pump, pipeline 17 is sent one-level wash water into crystallization kettle it is carried out to condensing crystal (being that one-level wash water carries out outer circulation), after removing hydrogenchloride, obtain 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 secondary pipeline static mixer jointly by pipeline 26, described chlorated liquid is fully mixed with secondary wash water, then mixed solution is through pipeline 22, secondary washing pump, pipeline 23 enters secondary washing separator and (hydrogenchloride in chlorated liquid and iron trichloride is extracted in secondary wash water, make secondary wash water contain acidity), the secondary chlorination liquid that outlet end flows out from secondary washing separator enters the liquid feeding end (entering third stage water-washing step) of triode road static mixer through pipeline 31, and secondary wash water outlet end from secondary washing separator 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 secondary pipeline static mixer, and and from the one-level chlorated liquid of one-level washing separator, again fully mix, like this, described secondary wash water carries out again and again in a manner described internal recycle in the washing equipment of the second stage, when the hydrogenchloride in secondary wash water and the weight percent concentration of iron trichloride reach 5%, by secondary wash water recycle pump, the upper liquid feeding end of one-level wash water circulation groove sent into secondary wash water by pipeline 27, described secondary wash water is reused (being that 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 triode road static mixer jointly by pipeline 36, described chlorated liquid is fully mixed with three grades of wash waters, then mixed solution is through pipeline 32, three grades of washing pumps, pipeline 33 enters three grades of washing separators and (hydrogenchloride in 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 outlet end from three grades of washing separators enters three grades of wash water circulation grooves automatically by pipeline 34, three grades of described wash waters are by pipeline 35, three grades of wash water recycle pumps, pipeline 36 enters in triode road static mixer, and and from the secondary chlorination liquid of secondary washing separator, again fully mix, like this, three grades of described wash waters carry out again and again in a manner described internal recycle in third stage washing equipment, when the hydrogenchloride in three grades of wash waters and the weight percent concentration of iron trichloride reach 1%, by three grades of wash water recycle pumps, the upper liquid feeding end of secondary wash water circulation groove sent into three grades of wash waters by pipeline 37, three grades of described wash waters are reused (three grades of wash waters carry out outer circulation) in the water-washing step of the second stage, meanwhile, by pipeline 39, in three grades of wash water circulation grooves, supplement water purification, separately, three grades of chlorated liquids that outlet end flows out from three grades of washing separators are delivered to chlorated liquid moisture eliminator by pipeline 38 and are carried out separation and be dried.
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 is only one embodiment of the present invention.It should be pointed out that for the person of ordinary skill of the art, under the premise without departing from the principles of the invention, can also make apparent some conversion or substitute 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, 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, this chlorated liquid is: purified petroleum benzin is by the effect of catalyzer, in chlorinator by chlorinated with chlorine, chlorated liquid after chloride process is acid and contains impurity, catalyzer is iron trichloride, and impurity comprises hydrogenchloride and iron trichloride.
2. the method for purification of chlorated liquid according to claim 1, it is characterized in that: when the hydrogenchloride in three grades of wash waters of third stage water-washing step and the weight percent concentration of iron trichloride reach 1%, three grades of wash waters are sent into second stage water-washing step, synchronously to third stage water-washing step, supplement water purification; When the hydrogenchloride in the secondary wash water of second stage water-washing step and the weight percent concentration of iron trichloride reach 5%, secondary wash water is sent into first step water-washing step; When the hydrogenchloride in the one-level wash water of first step water-washing step and the weight percent concentration of iron trichloride reach 10%, one-level wash water is sent into crystallization kettle it is carried out to condensing crystal, remove after hydrogenchloride to obtain solid phase iron trichloride.
3. the method for purification of chlorated liquid according to claim 1 and 2, is characterized in that: in every grade of water-washing step, be equipped with the pipeline static mixer that chlorated liquid and corresponding stage wash water are mixed.
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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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| CN102140055B true CN102140055B (en) | 2014-03-12 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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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