CN102698994B - Cleaning method of high-purity peroxyacetic acid production equipment and packing barrel - Google Patents
Cleaning method of high-purity peroxyacetic acid production equipment and packing barrel Download PDFInfo
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- CN102698994B CN102698994B CN201210186069.9A CN201210186069A CN102698994B CN 102698994 B CN102698994 B CN 102698994B CN 201210186069 A CN201210186069 A CN 201210186069A CN 102698994 B CN102698994 B CN 102698994B
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Abstract
The invention relates to a cleaning method of peroxyacetic acid production equipment and a packing barrel. The cleaning method comprises a cleaning process and a cleaning waste liquid disposal process, wherein the cleaning process is carried out according to a procedure comprising the following steps of: cleaning by using ultrapure water, drying by using purified air, soaking by using an ultrapure high-concentration peroxyacetic acid solution, cleaning by using the ultrapure water, drying by using the purified air, wherein the resistivity of the ultrapure water used for ultrapure water cleaning is higher than and equal to 18.0 M, and ultrapure high-concentration peroxyacetic acid solution soaking means that the peroxyacetic acid production equipment and the packing barrel are soaked by using 35-40 percent of the ultrapure high-concentration peroxyacetic acid solution by weight; and the cleaning waste liquid disposal process comprises the following step of: simultaneously preparing the ultrapure high-concentration peroxyacetic acid solution and a conventional high-concentration peroxyacetic acid solution by using waste peroxyacetic acid liquid generated through cleaning. According to the invention, the single impurity dissolution quantity of the peroxyacetic acid production equipment and the packing barrel which are cleaned through the cleaning method is lower than 5 ppb, and therefore, the production requirements and the storage requirements of high-purity peroxyacetic acids without additives are met; and in addition, the invention is integrally effective in process and environmental-friendly.
Description
Technical field
The invention belongs to the high purity peroxyacetic acid preparing technical field, particularly the cleaning method of a kind of high purity peroxyacetic acid production equipment and pail pack.
Background technology
Peracetic acid is colourless penetrating odor liquid, belongs to strong oxidizer, easily decompose, and under the conditions such as alkalescence, reducing substances and metal ion, vigorous reaction, decomposition or even blast.Peracetic acid is again good organic peroxide, in the many-side field that has a wide range of applications, it has efficient quick sterilization effect, multiple germs such as kill bacteria, gemma fungi, saccharomycete fast, thereby can be used as the disinfectant of infectious disease, drinking water, food etc.At SARS epidemic period, during the Wenchuan earthquake epidemic prevention, Peracetic acid has played significant role.Peracetic acid also has good oxidation susceptibility, can be used as organic synthesis oxidant, epoxidizing agent, polymerization initiator etc.Simultaneously, Peracetic acid also has been widely used in the fields such as desulfurization of bleaching, modification and the heavy oil of papermaking, textile industry.
At present, the industrial goods Peracetic acid requires the mass concentration of Peracetic acid > 15%.But meet at present the industry product Peracetic acid of this concentration requirement in storage and use procedure, the situation that decomposition of peracetic acid even explodes very easily occurs.According to the investigation of 2004 such as Wen Dongsheng of Shaanxi health monitoring institutions, 46 Peracetic acid manufacturing enterprises, the product of 60 batches, qualified 39 batches, qualification rate is only 65%.Different memory times, qualification rate is that 90.9%, 11 day qualification rate is 27.27% in three days, surpasses 20 days, all defective.According to just in July, 2003 investigation of the national Register of chemicals Li Yun of registration center, 1 to 12 May in 2003, more than 30 of Peracetic acid accident occurs in addition, dead 5 people, people more than 70 is poisoning or burn.In November, 2003, the blast of Yunnan Peracetic acid storage tank, 5 people's death, 4 buildings are burnt.Visible, the unstability of Peracetic acid has caused very adverse influence to economy and the security in its use procedure.Therefore, need to improve its stability and strengthen economy and the security in its storage and use procedure.
Domestic a lot of scholar, as Hao Wenhui, Ma Chunyu, Wang Lihua etc. have also noticed problems, also carried out trying to explore of related fields, makes some progress.But on the whole, effect is little, do not form extensive high stable property Peracetic acid Industrialized processing technique in batches.The production of our times main flow is to adopt to add the stability that stabilizing agent improves Peracetic acid.Yet, the additives such as use phosphorus not only increase the impurity content in Peracetic acid, make it can not be in sector applications such as biologic product, food, and the interpolation of the additive such as phosphorus, also can cause corrosion to equipment, reduce equipment life, cause other side reaction, accessory substance, also can make the eutrophication such as water body simultaneously, to environment.
The applicant finds through long-term practice and research, by (the individual event impurity metal ion content≤5ppb of the control to impurity ion content in peracetic acid soln, individual event anionic impurity content≤1ppm, organic impurities content≤5ppm) be expected to realize the stability of peracetic acid soln excellence, thereby avoid the interpolation of any stabilizer element, the one,, the peracetic acid soln product purity is higher, can be applied to the high-end fields such as medical treatment, food, biologic product, open up the application of Peracetic acid; The 2nd, it is applied in to the synthetic field of reagent, can reduce side reaction, reduce accessory substance, improve reaction yield; The 3rd,, because it is fully not phosphorous and part complex compound, chelate additive, make product have more environment friendly.
Peracetic acid is acid strong oxidizing property chemicals, very easily packaging material is caused to corrosion, and then forms various impurity strippings.Therefore, prepare the strict Peracetic acid product of controlling of impurity content and guarantee that in product, impurity content is not more big changes in storing process, except using highly purified raw materials, also must be controlled for the impurity stripping of the equipment used in the Peracetic acid production process and the Peracetic acid packing of product, otherwise be difficult to guarantee not contain the stability of the high purity peroxyacetic acid product of stabilizing agent, the useful life of product also will be very limited.
In prior art, what for Peracetic acid production equipment and pail pack, take is conventional water cleaning process, can't reach not containing the high purity peroxyacetic acid production of stabilizing agent and the requirement of packing.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and the cleaning method of a kind of high purity peroxyacetic acid production equipment and pail pack is provided.
For solving the problems of the technologies described above, the present invention takes following technical scheme:
The cleaning method of a kind of Peracetic acid production equipment and pail pack, described production equipment comprises reactor and pipeline, described cleaning method comprises matting and waste liquid disposal operation, wherein:
Described matting cleans → purifies air according to ultra-pure water and dry up → and ultrapure high concentration peroxy acid solution immersion → ultra-pure water cleans → purify air the flow process dried up to carry out, ultra-pure water cleans ultrapure resistivity of water used and is more than or equal to 18.0M Ω cm, the ultrapure peracetic acid soln that it is 35wt～40wt% that ultrapure high concentration peroxy acid solution immersion refers to by concentration is soaked described production equipment and pail pack, soak time is 24～36 hours, soaking temperature is room temperature, individual event impurity metal ion content≤5ppb in ultrapure peracetic acid soln, individual event anionic impurity content≤1ppm, organic impurities content≤5ppm,
Described waste liquid disposal operation comprises that the Peracetic acid waste liquid produced with cleaning prepares the step of ultrapure peracetic acid soln and conventional peracetic acid soln simultaneously, specifically comprises:
(1), make to clean the Peracetic acid waste liquid produce 40 ℃～50 ℃ of temperature, tower internal pressure 0.05～0.15atm rectification under vacuum, obtain Peracetic acid rectifying liquid and Peracetic acid distillation residual liquid;
(2) it is 2wt%～38wt% that the ultra-pure water that, step (1) gained Peracetic acid rectifying liquid is more than or equal to 18.0M Ω cm by resistivity is adjusted to concentration, with 0.1 micron filter core circulating filtration 0.5～3 hour, filling with through described matting, cleaning and detect qualified pail pack, obtain ultrapure peracetic acid soln;
(3), in step (1) gained Peracetic acid distillation residual liquid, add stabilizing agent, glacial acetic acid, the hydrogen peroxide that needs ratio, controlling Peracetic acid concentration is 5wt～22wt%, with 0.1 micron filter element filtering, filling, obtains conventional peracetic acid soln.
According to a concrete aspect of the present invention, described ultra-pure water cleans the cleaning way of taking spray, and during spray, pump pressure is 0.3～0.5MPa.The described pressure purified air that dries up use that purifies air is 0.3～0.6Mpa.
According to further embodiment of the present invention: described matting also comprises whether production equipment and pail pack after cleaning according to described flow process are cleaned to qualified detecting step.Preferably, the method that detecting step is taked is ultrapure resistivity of water after test cleaning production equipment or pail pack, and resistivity is more than or equal to 15M Ω cm, judges that cleaning is qualified; Otherwise, clean defectively, need repeated washing.
According to the present invention, above-mentioned reactor, pipeline and pail pack are known in the art.Preferably, reactor has the inner lining body that material is Kynoar; Pipeline has the inner lining body of material Kynoar or polytetrafluoroethylene (PTFE); The material of pail pack is high density polyethylene (HDPE).
The mentioned ultrapure resistivity of water of the present invention all refers to value measured under 25 ℃.The ultrapure resistivity of water that cleans use is more high better.In the suggestion actual production, ultrapure resistivity of water is 18.0～18.2M Ω cm.
Due to the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
Production equipment after cleaning according to cleaning method of the present invention and the individual event impurity stripping quantity of pail pack, lower than 5ppb, can meet the production requirement and the memory requirement that do not contain the high purity peroxyacetic acid of additive.In addition, cleaning method of the present invention, without any the waste of raw material, cleans high-purity high concentration peroxy acid of use after treatment, is prepared into again ultrapure peracetic acid soln product and conventional peracetic acid soln product, the whole effective and environmental protection of technique.
The specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the invention is not restricted to following examples.
Embodiment 1
The present embodiment provides a kind of cleaning method of the high-density polyethylene drum as high purity peroxyacetic acid solution pail pack, comprising:
1, matting:
At first the ultra-pure water spray irrigation pail pack that is 18.2M Ω cm by resistivity, drenching the flushing pump pressure is 0.4MPa, spray irrigation, after 3～5 minutes, dries up with the 0.4MPa purification of compressed air; Then by the filling 35wt% high purity peroxyacetic acid of pail pack solution, and after room temperature (approximately 20～25 ℃) stores 24 hours, Peracetic acid is drained, the ultra-pure water that is 18.2M by resistivity again cleans, purification of compressed air dries up standby, ultra-pure water after cleaning is detected, and wherein the individual event pollutant load is all lower than 5ppb.With the 35wt% peracetic acid soln, be stored in the pail pack after cleaning, 25 ℃ of storages 30 days, various Leaching rule amounts are lower than 5ppb.
2, clean the processing of the Peracetic acid waste liquid produced
(1) the Peracetic acid waste liquid produced in above-mentioned matting passes into the rectification under vacuum tower, rectifying, cooling water flow 5 ± 1L/h, steam pressure 0.01～0.05Mpa, feed rate 200 ± 50L/h, 45～50 ℃ of tower top temperatures, 0～5 ℃ of condenser and product temperature, obtain Peracetic acid rectifying liquid (approximately containing Peracetic acid 40%～50%) and Peracetic acid distillation residual liquid.
(2), by step (1) gained rectifying liquid, by resistivity, being 18.2M Ω cm, ultra-pure water is diluted to 35wt%, do ultrapure peracetic acid soln product and sell.After testing, do not contain hydrogen peroxide and acetic acid, individual event impurity metal ion content≤5ppb wherein, individual event anionic impurity content≤1ppm, organic impurities content≤5ppm in this product.
(3), step (1) gained Peracetic acid distillation residual liquid accounts for the 40wt% of total feed, wherein containing the Peracetic acid of the 6wt% that has an appointment and micro-hydrogen peroxide, glacial acetic acid.Glacial acetic acid content is added to 16%, and hydrogen peroxide concentration adds to 22wt%, adds the 0.1wt% stabilizing agent, obtains conventional peracetic acid soln (5wt%) product.
Embodiment 2
The present embodiment provides a kind of cleaning method of the high-density polyethylene drum as high purity peroxyacetic acid solution pail pack, comprising:
1, matting:
At first the ultra-pure water that is 18.2M Ω cm by resistivity, the spray irrigation pail pack, drenching the flushing pump pressure is 0.5MPa, spray irrigation, after 3～5 minutes, dries up with the 0.4MPa purification of compressed air; Then by the filling 37wt% high purity peroxyacetic acid of pail pack solution, and after room temperature (approximately 22～26 ℃) stores 24 hours, Peracetic acid is drained, the ultra-pure water that is 18.2M Ω cm by resistivity again cleans, purification of compressed air dries up standby, ultra-pure water after cleaning is detected, and wherein the individual event pollutant load is all lower than 5ppb.With the 35wt% peracetic acid soln, be stored in the pail pack after cleaning, 25 ℃ of storages 30 days, various Leaching rule amounts are lower than 5ppb.
2, clean the processing of the Peracetic acid waste liquid produced
(1) the Peracetic acid waste liquid produced in above-mentioned matting passes into the rectification under vacuum tower, rectifying, cooling water flow 5 ± 1L/h, steam pressure 0.01～0.05Mpa, feed rate 200 ± 50L/h, 45～50 ℃ of tower top temperatures, 0～5 ℃ of condenser and product temperature, obtain Peracetic acid rectifying liquid and Peracetic acid distillation residual liquid.
(2), by step (1) gained rectifying liquid, by resistivity, being 18.2M Ω cm, ultra-pure water is diluted to 35wt%, do ultrapure peracetic acid soln product and sell.After testing, do not contain hydrogen peroxide and acetic acid, individual event impurity metal ion content≤5ppb wherein, individual event anionic impurity content≤1ppm, organic impurities content≤5ppm in this product.
(3), step (1) gained distillation residual liquid accounts for the 30wt% of total feed, wherein containing the Peracetic acid of the 3wt% that has an appointment and micro-hydrogen peroxide, glacial acetic acid.Add wherein glacial acetic acid 22wt%, hydrogen peroxide 22wt%, stabilizing agent 0.1wt%, and again 40 ℃ the insulation 12 hours, obtain conventional peracetic acid soln product (5wt%).
Embodiment 3
The present embodiment provides the cleaning method of a kind of high purity peroxyacetic acid solution reaction still (the inner lining body material is Kynoar), comprising:
1, matting:
At first the ultra-pure water that is 15M Ω cm by resistivity, the spray irrigation reactor, drenching the flushing pump pressure is 0.5MPa, spray irrigation, after 5～10 minutes, dries up with the 0.5MPa purification of compressed air; Then by the filling 40wt% high purity peroxyacetic acid of reactor solution, and after room temperature (approximately 22～26 ℃) stores 24 hours, Peracetic acid is drained, the ultra-pure water that is 18.2M Ω cm by resistivity again cleans, purification of compressed air dries up standby, ultra-pure water after cleaning is detected, and wherein the individual event pollutant load is all lower than 5ppb.With the 35wt% peracetic acid soln, be stored in the pail pack after cleaning, 25 ℃ of storages 30 days, various Leaching rule amounts are lower than 5ppb.
2, clean the processing of the Peracetic acid waste liquid produced
(1) the Peracetic acid waste liquid produced in above-mentioned matting passes into the rectification under vacuum tower, rectifying, cooling water flow 5 ± 1L/h, steam pressure 0.01～0.05Mpa, feed rate 200 ± 50L/h, 45～50 ℃ of tower top temperatures, 0～5 ℃ of condenser and product temperature, obtain Peracetic acid rectifying liquid and Peracetic acid distillation residual liquid.
(2), by step (1) gained rectifying liquid, by resistivity, being 18.2M Ω cm, ultra-pure water is diluted to 35wt%, do ultrapure peracetic acid soln product and sell.After testing, do not contain hydrogen peroxide and acetic acid, individual event impurity metal ion content≤5ppb wherein, individual event anionic impurity content≤1ppm, organic impurities content≤5ppm in this product.
(3), step (1) gained distillation residual liquid accounts for 30～50% of total feed, wherein contain the Peracetic acid of the 8wt% that has an appointment, containing glacial acetic acid, hydrogen peroxide, add wherein glacial acetic acid 14wt%, hydrogen peroxide 20wt%, stabilizing agent 0.1wt% in addition, allocate and obtain conventional Peracetic acid 5wt% solution product.
Embodiment 4～6
Embodiment 4 to 6 provides respectively and has not contained the preparation method of the high purity peroxyacetic acid solution of stabilizing agent, specific as follows: as successively high-purity hydrogen peroxide (composition is referring to table 1) of 70% concentration and high-purity glacial acetic acid (composition is referring to table 2) to be squeezed in the reactor after embodiment 2 cleans according to the ratio of table 3, by mixed liquor at 45 ℃ of lower circular response 36h, the 0.1 micron filter filter core circulating filtration by routine, pail pack after cleaning with embodiment 1 is filling, obtains the peracetic acid soln product that does not contain stabilizing agent.This product after testing, individual event impurity metal ion content≤5ppb wherein, individual event anionic impurity content≤1ppm, organic impurities content≤5ppm.Stability to product is tested, and the content of Peracetic acid and hydrogen peroxide is also listed in table 3 over time.
The composition test result of the high-purity hydrogen peroxide of table 1
The composition test result of the high-purity glacial acetic acid of table 2
Table 3
Comparative Examples 1
This Comparative Examples provides a kind of preparation method who does not contain the high purity peroxyacetic acid solution of additive, its basic process is with embodiment 4～6, different is, its ratio listed according to table 3 adds high-purity hydrogen peroxide and high-purity glacial acetic acid, and the pail pack used of final product is that only to adopt resistivity be the pail pack after 18.2M Ω cm ultra-pure water cleans.
Comparative Examples 2
This Comparative Examples provides a kind of preparation method who does not contain the high purity peroxyacetic acid solution of additive, its basic process is with embodiment 4～6, different is, its ratio listed according to table 3 adds high-purity hydrogen peroxide and high-purity glacial acetic acid, and reactor wherein only adopted the ultra-pure water that resistivity is 18.2M Ω cm to clean before use.
As seen from Table 3, the stability that does not contain the high purity peroxyacetic acid solution product of additive that Comparative Examples 1 provides with 2 is compared with the stability of embodiment 4～6, obviously poor.
Above the present invention is described in detail; its purpose is to allow the personage who is familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence that all Spirit Essences according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention.
Above the present invention is described in detail; its purpose is to allow the personage who is familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence that all Spirit Essences according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention.
Claims (7)
1. the cleaning method of a high purity peroxyacetic acid production equipment and pail pack, described production equipment comprises reactor and pipeline, it is characterized in that: described cleaning method comprises matting and waste liquid disposal operation, wherein:
Described matting cleans → purifies air according to ultra-pure water and dry up → and ultrapure high concentration peroxy acid solution immersion → ultra-pure water cleans → purify air the flow process dried up to carry out, described ultra-pure water cleans ultrapure resistivity of water used and is more than or equal to 18.0M Ω cm, the ultrapure peracetic acid soln that it is 35wt～40wt% that described ultrapure high concentration peroxy acid solution immersion refers to by concentration is soaked described production equipment and pail pack, soak time is 24～36 hours, soaking temperature is room temperature, individual event impurity metal ion content≤5ppb in described ultrapure peracetic acid soln, individual event anionic impurity content≤1ppm, organic impurities content≤5ppm,
Described waste liquid disposal operation comprises that the Peracetic acid waste liquid produced with cleaning prepares the step of ultrapure peracetic acid soln and conventional peracetic acid soln simultaneously, specifically comprises:
(1), make to clean the Peracetic acid waste liquid produce 40 ℃～50 ℃ of temperature, tower internal pressure 0.05～0.15atm rectification under vacuum, obtain Peracetic acid rectifying liquid and Peracetic acid distillation residual liquid;
(2) it is 2wt%～38wt% that the ultra-pure water that, step (1) gained Peracetic acid rectifying liquid is more than or equal to 18.0M Ω cm by resistivity is adjusted to concentration, with 0.1 micron filter core circulating filtration 0.5～3 hour, filling with through described matting, cleaning and detect qualified pail pack, obtain ultrapure peracetic acid soln;
(3), in step (1) gained Peracetic acid distillation residual liquid, add stabilizing agent, glacial acetic acid, the hydrogen peroxide that needs ratio, controlling Peracetic acid concentration is 5wt～22wt%, with 0.1 micron filter element filtering, filling, obtains conventional peracetic acid soln.
2. the cleaning method of high purity peroxyacetic acid production equipment according to claim 1 and pail pack is characterized in that: described ultra-pure water cleans the cleaning way of taking spray, and during spray, pump pressure is 0.3～0.5MPa.
3. the cleaning method of high purity peroxyacetic acid production equipment according to claim 1 and pail pack, it is characterized in that: the described pressure purified air that dries up use that purifies air is 0.3～0.6Mpa.
4. the cleaning method of high purity peroxyacetic acid production equipment according to claim 1 and pail pack is characterized in that: described matting also comprises whether production equipment and pail pack after cleaning according to described flow process are cleaned to qualified detecting step.
5. the cleaning method of high purity peroxyacetic acid production equipment according to claim 4 and pail pack, it is characterized in that: the method that described detecting step is taked is ultrapure resistivity of water after test cleaning production equipment or pail pack, resistivity is more than or equal to 15M Ω cm, judges that cleaning is qualified; Otherwise, clean defectively, need repeated washing.
6. according to the cleaning method of the described high purity peroxyacetic acid production equipment of any one claim in claim 1 to 5 and pail pack, it is characterized in that: described reactor has the inner lining body that material is Kynoar; Described pipeline has the inner lining body that material is Kynoar or polytetrafluoroethylene (PTFE).
7. according to the cleaning method of the described high purity peroxyacetic acid production equipment of any one claim in claim 1 to 5 and pail pack, it is characterized in that: the material of described pail pack is high density polyethylene (HDPE).
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| CN107684687A (en) * | 2017-08-23 | 2018-02-13 | 江苏新美星包装机械股份有限公司 | A kind of retracting device and recovery method for peracetic acid disinfectant |
| CN107626699B (en) * | 2017-09-20 | 2020-04-24 | 宁德市凯欣电池材料有限公司 | Cleaning process for electrolyte barrel |
| CN112170411B (en) * | 2019-07-05 | 2024-01-12 | 长鑫存储技术有限公司 | Automatic cleaning and detecting device and method for carrier |
| TWI843303B (en) * | 2022-11-28 | 2024-05-21 | 關東鑫林科技股份有限公司 | Method for cleaning container of chemical product |
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| DE4342787C1 (en) * | 1993-12-15 | 1995-07-06 | Thiedig & Co Dr | Method for the quantitative determination of electrochemically reducible or oxidizable substances, in particular peroxyacetic acid in a mixture with other oxidizing substances |
| GB2277028B (en) * | 1993-12-24 | 1996-01-03 | Gw Chemicals Ltd | Cleaning beer dispense lines using peracetic acid |
| US7473323B2 (en) * | 1996-09-04 | 2009-01-06 | Maasland N.V. | Method and apparatus for cleaning a milk line system |
| US5977403A (en) * | 1997-08-04 | 1999-11-02 | Fmc Corporation | Method for the production of lower organic peracids |
| CN101781241A (en) * | 2010-01-18 | 2010-07-21 | 江苏爱利思达清泉化学有限公司 | Preparation method of anhydrous peroxyacetic acid |
| CN101804969A (en) * | 2010-04-02 | 2010-08-18 | 赫格雷(大连)制药有限公司 | Low-carbon environment friendly production method for extra high-purity H2O2 |
| CN102219722B (en) * | 2011-07-27 | 2013-10-30 | 上海哈勃化学技术有限公司 | Production technology of high purity peroxyacetic acid |
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| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 215000 No. 168, Shanfeng Road, Hedong Industrial Park, Wuzhong Economic Development Zone, Suzhou, Jiangsu Patentee after: Jingrui Electronic Materials Co.,Ltd. Address before: 215168 No. 3, Chenghu East Road, Wuzhong Economic Development Zone, Suzhou, Jiangsu Patentee before: SUZHOU CRYSTAL CLEAR CHEMICAL Co.,Ltd. |