CN114291799A - Production process of high-purity phosphorous acid - Google Patents
Production process of high-purity phosphorous acid Download PDFInfo
- Publication number
- CN114291799A CN114291799A CN202111551890.1A CN202111551890A CN114291799A CN 114291799 A CN114291799 A CN 114291799A CN 202111551890 A CN202111551890 A CN 202111551890A CN 114291799 A CN114291799 A CN 114291799A
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- CN
- China
- Prior art keywords
- hydrochloric acid
- tank
- reaction liquid
- kettle
- phosphorus trichloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 26
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002425 crystallisation Methods 0.000 claims abstract description 17
- 230000008025 crystallization Effects 0.000 claims abstract description 17
- 238000010521 absorption reaction Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000004821 distillation Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 230000005484 gravity Effects 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 238000011010 flushing procedure Methods 0.000 claims abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
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Abstract
The invention relates to a high-purity phosphorous acid production process, which comprises the following steps: the method comprises the following steps: adding metered hydrochloric acid into a dripping kettle, pumping phosphorus trichloride into a high-position metering tank from a phosphorus trichloride finished product tank, adding a proper amount of hydrochloric acid into the dripping tank, slowly dripping phosphorus trichloride into the dripping tank, controlling the temperature to be 60 +/-5 ℃, absorbing generated hydrochloric acid through a hydrochloric acid absorption tank, and absorbing and discharging the remaining tail gas into the external air through a water flushing pump; step two: after the phosphorus trichloride is added, the temperature is slowly raised to 90-95 ℃ through steam to remove a small amount of hydrochloric acid, the specific gravity of the reaction liquid is measured to be 1.4-1.5, the reaction liquid is sucked into a distillation kettle through vacuum, the negative pressure is raised to 128 +/-5 ℃, the reaction liquid is cooled to 108 +/-5 ℃ and is put into a crystallization kettle to be continuously cooled and crystallized, and after the crystallization exceeds 80%, the reaction liquid is put into a centrifuge to be centrifuged at high speed to obtain the finished phosphorous acid. The invention has the following advantages: the produced phosphorous acid has high purity and short production period.
Description
Technical Field
The invention relates to the technical field of phosphorous acid production, in particular to a high-purity phosphorous acid production process.
Background
Phosphorous acid is an oxyacid of phosphorus having the formula H3PO3The molecular weight is 82.00, the melting point is 74 ℃, the boiling point is 200 ℃, and the appearance is colorless crystal; the phosphorous acid is a dibasic acid, belongs to an inorganic compound, has slightly stronger acidity than phosphoric acid, has strong reducibility, is easy to reduce silver ions into metallic silver, can reduce sulfuric acid into sulfur dioxide, and has strong hygroscopicity, deliquescence and corrosivity; is easily dissolved in water and alcohol, is slowly oxidized into phosphoric acid in the air, and is decomposed into phosphine and phosphoric acid at 180 ℃.
The existing phosphorous acid production process has overlong production period, and the obtained phosphorous acid has low purity and can not meet the use requirement.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a high-purity phosphorous acid production process, which solves the problems in the background art.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a production process of high-purity phosphorous acid comprises the following steps:
the method comprises the following steps: adding metered hydrochloric acid into a dripping kettle, pumping phosphorus trichloride into a high-position metering tank from a phosphorus trichloride finished product tank, adding a proper amount of hydrochloric acid into the dripping tank, slowly dripping phosphorus trichloride into the dripping tank, controlling the temperature to be 60 +/-5 ℃, absorbing generated hydrochloric acid through a hydrochloric acid absorption tank, and absorbing and discharging the remaining tail gas into the external air through a water flushing pump;
step two: after the phosphorus trichloride is added, the temperature is slowly raised to 90-95 ℃ through steam to remove a small amount of hydrochloric acid, the specific gravity of the reaction liquid is measured to be 1.4-1.5, the reaction liquid is sucked into a distillation kettle through vacuum, the negative pressure is raised to 128 +/-5 ℃, the reaction liquid is cooled to 108 +/-5 ℃ and is put into a crystallization kettle to be continuously cooled and crystallized, and after the crystallization exceeds 80%, the reaction liquid is put into a centrifuge to be centrifuged at high speed to obtain the finished phosphorous acid.
As an improvement: in the first step, the pressure of the dropping kettle is less than 150 mmHg.
As an improvement: the pressure of the hydrochloric acid absorption tank in the first step is less than 50mmHg, and the temperature of the hydrochloric acid absorption tank in the first step is less than 50 ℃.
As an improvement: and the temperature of the crystallization kettle in the second step is 60 +/-5 ℃.
As an improvement: and in the second step, the pressure of the distillation kettle is-0.09 to 0.095 Mpa.
After the technical scheme is adopted, the invention has the beneficial effects that: the phosphorous acid produced by the process has high purity and short production period, and can meet the use requirement.
Drawings
Figure 1 is a flow diagram of a high purity phosphorous acid production process of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
The first embodiment is as follows: a production process of high-purity phosphorous acid comprises the following steps:
the method comprises the following steps: adding metered hydrochloric acid into a dropping kettle, wherein the pressure of the dropping kettle is 100mmHg, pumping phosphorus trichloride into a high-level metering tank from a phosphorus trichloride finished product tank, adding a proper amount of hydrochloric acid into the dropping tank, slowly dropping phosphorus trichloride into the dropping tank, controlling the temperature to be 55 ℃, absorbing generated hydrochloric acid through a hydrochloric acid absorption tank, controlling the pressure of the hydrochloric acid absorption tank to be 30mmHg and the temperature to be 30 ℃, and absorbing and discharging the rest tail gas into the external air through a water flushing pump;
step two: after the phosphorus trichloride is added, the temperature is slowly raised to 90 ℃ through steam to remove a small amount of hydrochloric acid, the specific gravity of the reaction liquid is measured to be 1.42, the reaction liquid is sucked into a distillation kettle through vacuum, the pressure of the distillation kettle is-0.09 Mpa, the negative pressure is raised to 123 ℃, the reaction liquid is cooled to 103 ℃, the reaction liquid is put into a crystallization kettle to be continuously cooled and crystallized, the temperature of the crystallization kettle is 55 ℃, and after the crystallization exceeds 80%, the reaction liquid is put into a centrifuge to be centrifuged at high speed to obtain the finished phosphorous acid.
Example two: a production process of high-purity phosphorous acid comprises the following steps:
the method comprises the following steps: adding metered hydrochloric acid into a dropping kettle, wherein the pressure of the dropping kettle is 100mmHg, phosphorus trichloride is pumped into a high-level metering tank from a phosphorus trichloride finished product tank, adding a proper amount of hydrochloric acid into the dropping tank, slowly dropping phosphorus trichloride into the dropping tank, controlling the temperature to be 60 ℃, absorbing generated hydrochloric acid through a hydrochloric acid absorption tank, controlling the pressure of the hydrochloric acid absorption tank to be 40mmHg and the temperature to be 35 ℃, and absorbing and discharging the rest tail gas into the external air through a water flush pump;
step two: after the phosphorus trichloride is added, slowly raising the temperature to 93 ℃ through steam to remove a small amount of hydrochloric acid, measuring the specific gravity of the reaction liquid to be 1.46, sucking the reaction liquid into a distillation kettle through vacuum, wherein the pressure of the distillation kettle is-0.092 Mpa, the negative pressure is raised to 128 ℃, cooling to 108 ℃, putting the reaction liquid into a crystallization kettle to continue cooling and crystallizing, the temperature of the crystallization kettle is 60 ℃, and after the crystallization exceeds 80%, putting the reaction liquid into a centrifuge to perform high-speed centrifugation to obtain the finished phosphorous acid.
Example three: a production process of high-purity phosphorous acid comprises the following steps:
the method comprises the following steps: adding metered hydrochloric acid into a dropping kettle, wherein the pressure of the dropping kettle is 100mmHg, pumping phosphorus trichloride into a high-level metering tank from a phosphorus trichloride finished product tank, adding a proper amount of hydrochloric acid into the dropping tank, slowly dropping phosphorus trichloride into the dropping tank, controlling the temperature to be 65 ℃, absorbing generated hydrochloric acid through a hydrochloric acid absorption tank, controlling the pressure of the hydrochloric acid absorption tank to be 20mmHg and the temperature to be 25 ℃, and absorbing and discharging the rest tail gas into the external air through a water flush pump;
step two: after the phosphorus trichloride is added, the temperature is slowly raised to 95 ℃ through steam to remove a small amount of hydrochloric acid, the specific gravity of the reaction liquid is measured to be 1.48, the reaction liquid is sucked into a distillation kettle through vacuum, the pressure of the distillation kettle is-0.094 Mpa, the negative pressure is raised to 133 ℃, the reaction liquid is cooled to 113 ℃, the reaction liquid is put into a crystallization kettle to be continuously cooled and crystallized, the temperature of the crystallization kettle is 65 ℃, and after the crystallization exceeds 80%, the reaction liquid is put into a centrifuge to be centrifuged at high speed to obtain the finished phosphorous acid.
The invention and its embodiments have been described above, without this being limitative. Without departing from the spirit of the invention, it is within the scope of the invention to suggest and appreciate that structural embodiments and examples similar to the technical solutions can be devised without inventing.
Claims (5)
1. A production process of high-purity phosphorous acid is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: adding metered hydrochloric acid into a dripping kettle, pumping phosphorus trichloride into a high-position metering tank from a phosphorus trichloride finished product tank, adding a proper amount of hydrochloric acid into the dripping tank, slowly dripping phosphorus trichloride into the dripping tank, controlling the temperature to be 60 +/-5 ℃, absorbing generated hydrochloric acid through a hydrochloric acid absorption tank, and absorbing and discharging the remaining tail gas into the external air through a water flushing pump;
step two: after the phosphorus trichloride is added, the temperature is slowly raised to 90-95 ℃ through steam to remove a small amount of hydrochloric acid, the specific gravity of the reaction liquid is measured to be 1.4-1.5, the reaction liquid is sucked into a distillation kettle through vacuum, the negative pressure is raised to 128 +/-5 ℃, the reaction liquid is cooled to 108 +/-5 ℃ and is put into a crystallization kettle to be continuously cooled and crystallized, and after the crystallization exceeds 80%, the reaction liquid is put into a centrifuge to be centrifuged at high speed to obtain the finished phosphorous acid.
2. The process according to claim 1 for the production of high purity phosphorous acid, wherein: in the first step, the pressure of the dropping kettle is less than 150 mmHg.
3. The process according to claim 1 for the production of high purity phosphorous acid, wherein: the pressure of the hydrochloric acid absorption tank in the first step is less than 50mmHg, and the temperature of the hydrochloric acid absorption tank in the first step is less than 50 ℃.
4. The process according to claim 1 for the production of high purity phosphorous acid, wherein: and the temperature of the crystallization kettle in the second step is 60 +/-5 ℃.
5. The process according to claim 1 for the production of high purity phosphorous acid, wherein: and in the second step, the pressure of the distillation kettle is-0.09 to 0.095 Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111551890.1A CN114291799A (en) | 2021-12-17 | 2021-12-17 | Production process of high-purity phosphorous acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111551890.1A CN114291799A (en) | 2021-12-17 | 2021-12-17 | Production process of high-purity phosphorous acid |
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| Publication Number | Publication Date |
|---|---|
| CN114291799A true CN114291799A (en) | 2022-04-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202111551890.1A Pending CN114291799A (en) | 2021-12-17 | 2021-12-17 | Production process of high-purity phosphorous acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115285953A (en) * | 2022-07-04 | 2022-11-04 | 泰州市永昌化工有限公司 | Phosphorus trichloride hydrolysis preparation process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5147625A (en) * | 1990-08-16 | 1992-09-15 | Hoechst Aktiengesellschaft | Process for the preparation of phosphorous acid |
| CN101993051A (en) * | 2009-08-21 | 2011-03-30 | 北京紫光英力化工技术有限公司 | Method for preparing phosphorous acid and hydrogen chloride |
| CN102249202A (en) * | 2011-06-16 | 2011-11-23 | 江苏大明科技有限公司 | Preparation process for synthesizing phosphorous acid by hydrolyzing phosphorous trichloride |
| CN104140081A (en) * | 2013-05-09 | 2014-11-12 | 新沂市汉菱生物工程有限公司 | Byproduct hydrochloric acid production method |
| CN104140087A (en) * | 2013-05-09 | 2014-11-12 | 新沂市汉菱生物工程有限公司 | Orthophosphorous acid production method |
-
2021
- 2021-12-17 CN CN202111551890.1A patent/CN114291799A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5147625A (en) * | 1990-08-16 | 1992-09-15 | Hoechst Aktiengesellschaft | Process for the preparation of phosphorous acid |
| CN101993051A (en) * | 2009-08-21 | 2011-03-30 | 北京紫光英力化工技术有限公司 | Method for preparing phosphorous acid and hydrogen chloride |
| CN102249202A (en) * | 2011-06-16 | 2011-11-23 | 江苏大明科技有限公司 | Preparation process for synthesizing phosphorous acid by hydrolyzing phosphorous trichloride |
| CN104140081A (en) * | 2013-05-09 | 2014-11-12 | 新沂市汉菱生物工程有限公司 | Byproduct hydrochloric acid production method |
| CN104140087A (en) * | 2013-05-09 | 2014-11-12 | 新沂市汉菱生物工程有限公司 | Orthophosphorous acid production method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115285953A (en) * | 2022-07-04 | 2022-11-04 | 泰州市永昌化工有限公司 | Phosphorus trichloride hydrolysis preparation process |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220408 |
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