CN103523756B - Production method of high-concentration hydrogen peroxide and device - Google Patents
Production method of high-concentration hydrogen peroxide and device Download PDFInfo
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- CN103523756B CN103523756B CN201310500973.7A CN201310500973A CN103523756B CN 103523756 B CN103523756 B CN 103523756B CN 201310500973 A CN201310500973 A CN 201310500973A CN 103523756 B CN103523756 B CN 103523756B
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Abstract
A kind of production method of high-concentration hydrogen peroxide, provides a kind of method being prepared high dense hydrogen peroxide product by hydrogen peroxide obtained by anthraquinone process solution, provides a kind of device for the method simultaneously.Adopt two cover production equipment continuous seepage, first by resin bed to hydrogen peroxide removal organism, then enter two cover production equipments, the production method of often overlapping production equipment includes following steps: the step that a. evaporates hydrogen peroxide; B. hydrogen peroxide is carried out to the step of gas-liquid separation; C. upper step gained gas phase is carried out to the step of rectifying; D. obtain hydrogen peroxide solution after the rectifying of upper step and reclaim.This production equipment comprises resin bed, still kettle, gas-liquid separator, rectifying tower and reflux ratio device and connecting pipeline, it is characterized in that: described gas-liquid separator and rectifying tower are packing tower.Its beneficial effect is: adopt the device continuous seepage that two covers are identical, technique is simple, and easily control, products obtained therefrom purity is high.
Description
Technical field:
The invention provides a kind of method being prepared high dense hydrogen peroxide product by hydrogen peroxide obtained by anthraquinone process solution, a kind of device for the method is provided simultaneously.
Background technology:
Hydrogen peroxide manufacture method is generally anthraquinone.In anthraquinone production, producing H2O2 is with 2-ethyl-anthraquinone (EAQ) for carrier, and heavy aromatics and trioctyl phosphate (TOP) are mixed solvent, is mixed with the solution (hereinafter referred to as working fluid) with definite composition.Working fluid enters and is equipped with in the hydrogenation tower of palladium catalyst together with hydrogen, under certain pressure and temperature, carry out hydrogenation, obtains corresponding 2-ethyl hydrogen anthraquinone (HEAQ) solution (hereinafter referred to as hydride).Hydride is again by the dioxygen oxidation in air, and the hydrogen anthraquinone in solution generates anthraquinone again, and simultaneous reactions produces H2O2.With pure water extraction containing H
2o
2working fluid (hereinafter referred to as oxidation solution), obtain H
2o
2the aqueous solution (being commonly called as hydrogen peroxide).H
2o
2the aqueous solution through heavy aromatics purifying treatment and air purge, the H2O2 product that concentration is 27.5% can be obtained, usually containing organic carbon at 50mg/kg to 200mg/kg.
In production method in the past, superoxol flashes to gas phase and with misty liquid droplets in vaporizer, in gas-liquid separator, misty liquid droplets is not separated well, and with some impurity in misty liquid droplets, except the inorganic acrobatics of apparatus surface, pipeline etc., misty liquid droplets will be solved from the design of Production Flow Chart and equipment the impact of quality product.
Summary of the invention:
The invention provides a kind of for from 27.5%(w/w) Purifying Hydrogen Peroxide and rectifying to 60%-65%(w/w), and then further by 60%-65%(w/w) hydrogen peroxide is concentrated to 90%-95%(w/w) method and apparatus, in order to achieve the above object, the technical solution used in the present invention is:
A kind of production method of high-concentration hydrogen peroxide, it is characterized in that production equipment continuous seepage is overlapped in employing two, first by resin bed to hydrogen peroxide removal organism, then enter two cover production equipments, the production method of often overlapping production equipment includes following steps: the step that a. evaporates hydrogen peroxide; B. hydrogen peroxide is carried out to the step of gas-liquid separation; C. upper step gained gas phase is carried out to the step of rectifying; D. obtain hydrogen peroxide solution after the rectifying of upper step and reclaim.
The vacuum tightness of above-described separating step is 3kPa-5.3kPa.
The temperature of above-described separating step is 40 DEG C-75 DEG C.
A kind of high-strength hydrogen peroxide production equipment, comprises resin bed, still kettle, gas-liquid separator, rectifying tower and reflux ratio device and connecting pipeline, it is characterized in that: described gas-liquid separator and rectifying tower are packing tower.
The height of above-described separator filler and garden column diameter are than being 1.5:1.
The height of above-described separator filler and garden column diameter are than being 1.2:1.
The packed height of above-described rectifying tower and rectifying tower diameter are than being 8:1.
The packed height of above-described rectifying tower and rectifying tower diameter are than being 6:1.
The reflux ratio of above-described rectifying tower is 1:4 to 4:1.
The invention has the beneficial effects as follows: adopt the device continuous seepage that two covers are identical, technique is simple, and easily control, products obtained therefrom purity is high.
Accompanying drawing illustrates:
Fig. 1 is the schema of production equipment of the present invention.
In figure: 1. rectifying tower; 2. resin bed; 3. purify storage tank; 4. still kettle; 5. condenser; 6. reflux ratio device; 7. lime set receiving tank; 8. storage tank; 9. separator.
Embodiment:
The invention provides a kind of for from 27.5%(w/w) Purifying Hydrogen Peroxide and rectifying to 60%-65%(w/w), and then further by 60%-65%(w/w) hydrogen peroxide is concentrated to 90%-95%(w/w) method and apparatus of (note: the concentration that the present invention mentions all refers to mass percent).See accompanying drawing 1, the superoxol of 27.5% flows into from the top of resin bed 2, flow into after removing most of organic carbon of hydrogen peroxide with resin effect and purify storage tank 3, superoxol after purification enters in still kettle 4, by steam or hot water by lipid peroxidation hydrogen-gasified, the phase hydrogen peroxide entered arrives bottom separator 9 from separator 9 top through packing layer, pass through packing layer after gas phase diffusion and in separator 9, misty liquid droplets removed, liquid phase flows back in still kettle 4, gas phase enters in rectifying tower 1 carries out rectifying, with the water of condensation that rectifying tower 1 top vapor condensation is out containing below hydrogen peroxidase 10 .1% by overhead condenser 5, water of condensation enters lime set receiving tank 7 by reflux ratio device 6 part, another part is got back in rectifying tower 1 as phegma, the intermediates that rectifying tower 1 bottom obtains rectifying flow into storage tank 8, for the superoxol of 60%-65%.
The 60%-65% superoxol obtained after rectifying enters in the still kettle 4 of the second cover rectifying tower by storage tank 8, in the second cover rectifier unit, further 60%-65% superoxol is concentrated to 90%-95% superoxol.Rectifying completes all under vacuo with concentrated, and the vacuum tightness of apparatus system is within the scope of 3kPa-5.3kPa, and the temperature of separator 9 ingress is within the scope of 40 DEG C-75 DEG C.
The product that this production equipment is produced, through adjustment content, can reach the standard of SILVER REAGENT hydrogen peroxide, food grade hydrogen peroxide, pharmaceutical grade hydrogen peroxide, and can produce the hydrogen peroxide of 90% concentration.
In Fig. 1, the filler material of separator 9 is stainless steel, can adopt structure formation general in chemical engineering, and the equipment size of rectifying tower 1 can calculate by engineering method, is not described in detail here.
In first set rectifying device, with 27.5% ~ 35% hydrogen peroxide for raw material, remove by the purification of resin bed the organism contained in hydrogen peroxide, adjustment acidity and stability reach processing requirement index.With vacuum by pipeline by purification after hydrogen peroxide suction still kettle 4 in, after the hot water heating of 95 DEG C-98 DEG C, hydrogen peroxide is vaporized, hydrogen peroxide after vaporization enters from separator 9 top through pipeline, and arrive bottom separator 9 after packing layer, after parting liquid pearl, through packing layer by separator 9 top out, enter in rectifying tower 1 through pipeline, the liquid phase in separator 9 is returned in still kettle 4.Separator 9 top vacuum tightness is within the scope of 3kPa-5.3kPa, the temperature of separator 9 ingress is within the scope of 40 DEG C-75 DEG C, enter the hydrogen peroxide in rectifying tower 1 and the phegma in reflux ratio device 6 carries out gas-liquid exchange, heavy component post liquefaction flows out rectifying tower 1 through pipeline and enters storage tank 8, product in the middle of the 60%-65% superoxol that this heavy component obtains after being rectifying, adjust in this material suction preparing tank (not shown), be reagent hydrogen peroxide or the raw material as the second cover rectifier unit.
Light ends by rectifying tower 1 top out, condenser 5 is entered through pipeline, vapour phase water condensation is made by recirculated cooling water at this, water of condensation is containing hydrogen peroxidase 10 .03%, water of condensation enters reflux ratio device 6 through pipeline, a part enters rectifying tower 1 as phegma, and another part enters lime set receiving tank 7 through pipeline and reclaims use.
Before concentration of hydrogen peroxide in still kettle 4 does not reach 70% ~ 75%, rectifying tower 1 does not reclaim middle product or finished product, and through pipeline total reflux in still kettle 4, now control of reflux ratio is between 1:4 to 1:1.After concentration of hydrogen peroxide reaches 70% ~ 75%, rectifying tower 1 reclaims middle product or finished product, and now control of reflux ratio is between 1:1 to 4:1.The adjustment of reflux ratio, with still kettle 4 endoperoxides hydrogen concentration for foundation, adjusts in above-mentioned scope.
50ml sample is got in the stability requirement of the hydrogen peroxide in still kettle 4, and when 96 DEG C, hydrogen peroxide is no more than 42ml at the decomposition amount of 1 hour.Otherwise, the feed liquid in still kettle 4 be changed.
In the second cover rectifying device, the hydrogen peroxide obtained with first set rectifying device concentrates for raw material, and adjustment acidity and stability reach processing requirement index.By vacuum by pipeline by hydrogen peroxide suction still kettle 4, after the hot water heating of 95 DEG C-98 DEG C, hydrogen peroxide is vaporized, hydrogen peroxide after vaporization enters from separator 9 top through pipeline, and arrive bottom separator 9 after packing layer, after parting liquid pearl, through packing layer by separator 9 top out, enter in rectifying tower 1 through pipeline, the liquid phase in separator 9 is returned in still kettle 4.Separator 9 top vacuum tightness is within the scope of 3kPa-5.3kPa, the temperature at separator inlet place is within the scope of 40 DEG C-75 DEG C, the hydrogen peroxide entered in rectifying tower 1 carries out gas-liquid exchange with the phegma returned in liquor ratio device 6, heavy component post liquefaction flows out rectifying tower 1 through pipeline, the 90%-95% superoxol finished product that this heavy component obtains after being and concentrating, the qualified input packaging process of sample examination, is high dense hydrogen peroxide.
Light ends by rectifying tower 1 top out, condenser 5 is entered through pipeline, vapour phase water condensation is made by recirculated cooling water at this, water of condensation is containing hydrogen peroxidase 10 .04%, water of condensation enters reflux ratio device 6 through pipeline, a part enters rectifying tower 1 as phegma, and another part enters lime set receiving tank 7 through pipeline and reclaims use.
50ml sample is got in the stability requirement of the hydrogen peroxide in still kettle 4, and when 96 DEG C, hydrogen peroxide is no more than 42ml at the decomposition amount of 1 hour.Otherwise, the feed liquid in still kettle be changed.
Claims (2)
1. a production method of high-concentration hydrogen peroxide, it is characterized in that: the Purifying Hydrogen Peroxide from 27.5% rectifying are to 60%-65%, and then further 60%-65% hydrogen peroxide is concentrated to 90%-95%, adopt two cover production equipment continuous seepage, first by resin bed to hydrogen peroxide removal organism, then enter two cover production equipments, the production method of often overlapping production equipment includes following steps: the step that a. evaporates hydrogen peroxide; B. hydrogen peroxide is carried out to the step of gas-liquid separation; C. upper step gained gas phase is carried out to the step of rectifying; D. obtain hydrogen peroxide solution after the rectifying of upper step and reclaim; The vacuum tightness of described separating step is 3kPa-5.3kPa; The temperature of described separating step is 40 DEG C-75 DEG C.
2. a device for production method of high-concentration hydrogen peroxide as claimed in claim 1, comprises resin bed, still kettle, gas-liquid separator, rectifying tower and reflux ratio device and connecting pipeline, it is characterized in that: described gas-liquid separator and rectifying tower are packing tower; The height of described separator filler and body diameter are than being 1.5:1; The packed height of described rectifying tower and rectifying tower diameter are than being 8:1; The reflux ratio of described rectifying tower is 1:4 to 4:1.
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| CN201310500973.7A CN103523756B (en) | 2013-10-23 | 2013-10-23 | Production method of high-concentration hydrogen peroxide and device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310500973.7A CN103523756B (en) | 2013-10-23 | 2013-10-23 | Production method of high-concentration hydrogen peroxide and device |
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| CN103523756A CN103523756A (en) | 2014-01-22 |
| CN103523756B true CN103523756B (en) | 2015-12-09 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203079B (en) * | 2016-12-16 | 2021-06-01 | 中国石油化工股份有限公司 | Hydrogen peroxide concentration device |
| KR102512609B1 (en) * | 2017-02-22 | 2023-03-21 | 미츠비시 가스 가가쿠 가부시키가이샤 | Manufacturing method and manufacturing system of purified aqueous hydrogen peroxide solution |
| CN109231173A (en) * | 2018-10-17 | 2019-01-18 | 杭州电化集团有限公司 | High-purity hydrogen peroxide preparation method and purification system |
| CN115259098A (en) * | 2022-08-24 | 2022-11-01 | 菏泽市巨丰新能源有限公司 | Method for continuously producing hydrogen peroxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257827A (en) * | 1998-12-21 | 2000-06-28 | 化学工业部黎明化工研究院 | Process for refining and concentrating hydrogen peroxide obtained by anthraquinone process |
| CN102757019A (en) * | 2012-06-14 | 2012-10-31 | 天津大学 | System and method for concentrating and purifying hydrogen peroxide |
| CN103204476A (en) * | 2013-04-08 | 2013-07-17 | 安徽晋煤中能化工股份有限公司 | Concentration-rectification optimized production system for concentrating 27.5% hydrogen peroxide dilute solution into 50% hydrogen peroxide thick solution and method thereof |
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2013
- 2013-10-23 CN CN201310500973.7A patent/CN103523756B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257827A (en) * | 1998-12-21 | 2000-06-28 | 化学工业部黎明化工研究院 | Process for refining and concentrating hydrogen peroxide obtained by anthraquinone process |
| CN102757019A (en) * | 2012-06-14 | 2012-10-31 | 天津大学 | System and method for concentrating and purifying hydrogen peroxide |
| CN103204476A (en) * | 2013-04-08 | 2013-07-17 | 安徽晋煤中能化工股份有限公司 | Concentration-rectification optimized production system for concentrating 27.5% hydrogen peroxide dilute solution into 50% hydrogen peroxide thick solution and method thereof |
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