CN1198402A - Telchnological process of sodium method producing bleaching powder extract - Google Patents
Telchnological process of sodium method producing bleaching powder extract Download PDFInfo
- Publication number
- CN1198402A CN1198402A CN 97103581 CN97103581A CN1198402A CN 1198402 A CN1198402 A CN 1198402A CN 97103581 CN97103581 CN 97103581 CN 97103581 A CN97103581 A CN 97103581A CN 1198402 A CN1198402 A CN 1198402A
- Authority
- CN
- China
- Prior art keywords
- mother liquor
- filter cake
- bleaching powder
- wet filter
- chlorine gas
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 52
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000007844 bleaching agent Substances 0.000 title claims abstract description 21
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title abstract description 8
- 239000011734 sodium Substances 0.000 title abstract description 8
- 229910052708 sodium Inorganic materials 0.000 title abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 40
- 239000012452 mother liquor Substances 0.000 claims abstract description 31
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000460 chlorine Substances 0.000 claims abstract description 29
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 17
- 239000012065 filter cake Substances 0.000 claims abstract description 17
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 13
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 13
- 239000004571 lime Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 12
- 239000012295 chemical reaction liquid Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910001868 water Inorganic materials 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 4
- 238000010586 diagram Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 abstract description 3
- 235000014483 powder concentrate Nutrition 0.000 abstract 2
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910001902 chlorine oxide Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- Paper (AREA)
Abstract
The preparation process fr producing bleaching powder concentrate by using sodium method includes the following steps: 1. chlorinating lime slurry to obtain wet filter cake and mother liquor A; 2. chlorinating the slurry liquor made up by using sodium hydroxide and mother liquor B to obtain sodium hypochlorite solution; 3. chlorinating the slurry liquor made up by mixing the wet filter cake with sodium hypochlorite solution to produce tetragonal lamellar crystal, then obtaining wet filter cake and mother liquor B, and after the wet filter cake is dried, obtaining the bleaching powder concentrate whose effective chlorine content is greater than or equal to 70%. The mother liquor A and mother B can be respectively circularly used. Said invention has the advantages of low cost, large crystal grain size, simple technological condition and definite end point of reaction.
Description
The invention relates to a process method for producing bleaching powder extract by a sodium method.
Bleaching powder, generally called bleaching powder, is a mixed crystal of calcium hypochlorite, calcium hydroxide and water, and the effective component of the bleaching powder is calcium hypochlorite. The quality of the bleaching powder is expressed by the content of available chlorine, and the bleaching powder with the chlorine content of more than or equal to 70 percent produced at present must be prepared by the reaction of calcium hydroxide, sodium hydroxide and chlorine, which is called as a sodium method. US367.2091(1983) discloses a sodium process which is mainly characterized by firstly chlorinating lime slurry and part of circulating mother liquor to produce calcium hypochlorite and calcium hydroxide crystals, filtering out solid impurities, adding alkali liquor and then chlorinating, and the above process has the following disadvantages: 1. high quality lime is required; 2. the reaction conditions are complex, strict requirements are imposed on the speed, concentration gradient, stirring mode and the like of chlorine, and the end point is difficult to control; 3. the generated crystals are small and are not easy to filter; 4. the consumption of sodium hydroxide and chlorine is high.
The invention aims to provide a process method for producing bleaching powder extract by a sodium method aiming at the defects of the prior art, wherein the bleaching powder extract with different effective chlorine contents has different crystal shapes to generate the bleaching powder extract with different crystal shapes according to the principle that corresponding solution composition is needed.
The invention aims to realize the technical method for producing the bleaching powder essence by the sodium method, which is characterized in that 1, lime slurry with the concentration of 25-35% (density of 115-125 g/100 ml) is used, chlorine is introduced at the temperature of below 65% until the effective chlorine content of crystals generated in the solution reaches 25-35%, the chlorine introduction is stopped, and the obtained reaction liquid is filtered to obtain a wet filter cake and a mother liquid ①, wherein the reaction process comprises the following steps:
2. according to the process flow chart 1, taking a mother solution ② and sodium hydroxide, wherein the ratio of the mother solution ② to the NaoH is 8: 1-1.5, uniformly mixing, and introducing chlorine gas at the temperature of below 30 ℃ to prepare a sodium hypochlorite solution, wherein the reaction process comprises the following steps:
filtering the solution obtained by the reaction, discarding the filter residue to obtain sodium hypochlorite (N)aOCl) solution for standby;
3. mixing the filter cake obtained in the process 1 and the sodium hypochlorite solution obtained in the process 2 according to the ratio of 0.8-1.5: 4 for pulping, introducing chlorine gas at the temperature of 10-20 ℃ until tetragonal flaky crystals are generated, stopping introducing chlorine, filtering the reaction product to obtain a wet filter cake and a mother liquor ②, and drying the wet filter cake to obtain bleaching powder with the effective chlorine content of more than or equal to 70%;
wherein the supernatant of the mother liquor ① is recycled in the process 1 or the process 2, and the mother liquor ② is recycled in the process 2.
Compared with the prior art, the method has the advantages that 1, the method adopts step-by-step chlorination, so that strict requirements on chlorine introducing speed, concentration gradient of chlorine in a reactor and reaction temperature are not required, process conditions are simple and easy to control, 2, the reaction end point can be observed clearly due to large crystal particles generated by the method, 3, the method reduces the consumption of chlorine and sodium hydroxide on solution generation conditions due to cyclic use of the mother liquor ① and the mother liquor ②, so that the production cost is reduced, 4, the content of insoluble substances in water in products produced by the method is low and is generally below 3%, and 5, the bleached powder obtained by the method has large crystal particles and is easy to filter.
The invention is described in detail below in the context of a preferred embodiment of the process according to the invention with reference to the process flow diagram:
FIG. 1 is a process flow diagram of the process of the present invention;
according to the figure 1, common chemical lime is adopted, and calcium hydroxide obtained after lime slaking and air separation is prepared into lime slurry for standby;
1. taking 1200 g of the lime slurry (the density is 118 g/100 ml), introducing chlorine gas at the temperature of below 65 ℃, stopping introducing the chlorine gas when the available chlorine content of crystals generated in the reaction liquid reaches 30 percent, wherein the chlorine introducing time is about 50 minutes, the weight of the reaction liquid is increased by 200 g, filtering to obtain 429 g of wet filter cake, the available chlorine content of the obtained mother liquor ① is 4.6 percent, and standing the mother liquor ①;
2.② 800 g of mother liquor is taken, 128 g of sodium hydroxide is added, after uniform mixing, chlorine is introduced at the temperature below 30 ℃, when the reaction solution becomes clear from turbidity and regular hexahedron crystals of sodium chloride are generated, the introduction of chlorine is stopped, the reaction solution is filtered, filter residue with the main content of sodium chloride is discarded, and the mother liquor is sodium hypochlorite solution for later use;
3. taking 250 g of the wet filter cake obtained in the process 1, adding 1000 g of the sodium hypochlorite solution obtained in the process 2, mixing with water, pulping, introducing chlorine below 30 ℃, stopping introducing the chlorine when tetragonal flaky crystals are generated in the reaction liquid, increasing the weight of the reaction liquid by 85 g, reacting for about 30 minutes, filtering the obtained reaction liquid to obtain 320 g of the wet filter cake and ② of mother liquor, wherein the effective chlorine content of the wet filter cake is 54.9%, the effective chlorine content of the mother liquor ② is 11.3%, drying the wet filter cake to obtain 217 g of the product bleaching powder, the effective chlorine content is 76.63%, and the content of water insoluble substances is 2.87%.
And (3) taking supernatant of the standing mother liquor ① for recycling in the process 1, recycling the mother liquor ② in the process 2, and adding water or diluting the supernatant of the mother liquor ① in the use process of the mother liquor ②.
The method adopts the process method of chlorination step by step and recycling mother liquor, and soluble impurities and insoluble impurities can be removed in the process 1, so high-quality lime is not needed, and the production requirement can be met by using common chemical lime.
The following table shows the data (unit: ton) of sodium hydroxide and chlorine gas consumed by the process of the present invention and the existing process according to the experimental results for producing one ton of bleaching powder with an available chlorine content of not less than 70%
Italy D of the south China sea chemical planteNore
The method of the invention
Chlorine consumption 0.9681.131.10 sodium hydroxide consumption 0.410.640.60 of caustic soda lime method and caustic soda lime method
From the above data, it can be seen that the consumption of sodium hydroxide and chlorine gas is reduced by the method, and the prices of the two raw materials are higher, so the production cost can be reduced by the method of the present invention.
Claims (4)
1. A, using lime slurry with the concentration of 25-35% (the density is 115-125 g/100 ml), introducing chlorine gas at the temperature below 65 ℃, stopping introducing the chlorine gas when the content of available chlorine of crystals generated in reaction liquid is 25-35%, and filtering the obtained reaction liquid to obtain a wet filter cake and mother liquid ①;
b. according to the process flow diagram 1, taking mother liquor ② and sodium hydroxide, wherein the ratio of the mother liquor ② to the sodium hydroxide is 8: 1-1.5, uniformly mixing, introducing chlorine gas at the temperature below 30 ℃ to obtain sodium hypochlorite solution, filtering the reaction solution, and removing filter residues to obtain mother liquor for later use;
c. mixing the wet filter cake obtained in the technological process a and the sodium hypochlorite solution obtained in the technological process according to the proportion of 0.8-1.5: 4, adding water for pulping, introducing chlorine gas at the temperature of 10-20 ℃ until orthohexagonal flaky crystals are generated, stopping introducing the chlorine gas, filtering the reaction liquid to obtain a wet filter cake and mother liquor ②, and filtering the obtained wet filter cake to obtain a bleaching powder product with the effective chlorine content of more than or equal to 70%;
wherein, after the mother liquor ① is stood still, supernatant liquor of the mother liquor is taken to be recycled in the process a, and the mother liquor ② is recycled in the process b.
2. A process for producing bleaching powder according to claim 1, wherein the introduction of chlorine gas is stopped when the reaction solution is clarified by turbidity and crystals of sodium chloride in regular tetrahedron are produced during the process b.
3. A process for producing bleaching powder according to claim 1, wherein the optimum ratio of wet cake to mother liquor ② obtained in process a used in process c is 1: 4.
4. A process for the production of bleaching powder according to claim 1 wherein the mother liquor ② is diluted with water or supernatant of the mother liquor ① during recycling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103581A CN1047573C (en) | 1997-05-04 | 1997-05-04 | Telchnological process of sodium method producing bleaching powder extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103581A CN1047573C (en) | 1997-05-04 | 1997-05-04 | Telchnological process of sodium method producing bleaching powder extract |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1198402A true CN1198402A (en) | 1998-11-11 |
| CN1047573C CN1047573C (en) | 1999-12-22 |
Family
ID=5166746
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97103581A Expired - Fee Related CN1047573C (en) | 1997-05-04 | 1997-05-04 | Telchnological process of sodium method producing bleaching powder extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1047573C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100424006C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
| CN100424005C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
| CN102101652A (en) * | 2010-04-30 | 2011-06-22 | 汪晋强 | Method for producing calcium chlorate and co-producing fine calcium carbonate and sodium chloride by using carbide slag |
| CN101646627B (en) * | 2007-03-28 | 2012-11-14 | 荷兰联合利华有限公司 | Water purification system |
| CN103342345A (en) * | 2013-07-15 | 2013-10-09 | 天津市郁峰化工有限公司 | Method for producing calcium hypochlorite by using sodium method |
| CN104355293A (en) * | 2014-10-22 | 2015-02-18 | 张世军 | Technology of utilizing sodium method to prepare calcium hypochlorite |
| CN105236355A (en) * | 2015-09-25 | 2016-01-13 | 广西大学 | Clean and environmental-protection bleaching powder production process |
| CN109336056A (en) * | 2018-11-20 | 2019-02-15 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of method for preparing calcium hypochlorite by sodium method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5293694A (en) * | 1976-02-03 | 1977-08-06 | Toyo Soda Mfg Co Ltd | Production of high test bleaching powder |
| US4399117A (en) * | 1982-02-04 | 1983-08-16 | Olin Corporation | Production of neutral calcium hypochlorite from its dibasic salt |
-
1997
- 1997-05-04 CN CN97103581A patent/CN1047573C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100424006C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
| CN100424005C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
| CN101646627B (en) * | 2007-03-28 | 2012-11-14 | 荷兰联合利华有限公司 | Water purification system |
| CN102101652A (en) * | 2010-04-30 | 2011-06-22 | 汪晋强 | Method for producing calcium chlorate and co-producing fine calcium carbonate and sodium chloride by using carbide slag |
| CN103342345A (en) * | 2013-07-15 | 2013-10-09 | 天津市郁峰化工有限公司 | Method for producing calcium hypochlorite by using sodium method |
| CN104355293A (en) * | 2014-10-22 | 2015-02-18 | 张世军 | Technology of utilizing sodium method to prepare calcium hypochlorite |
| CN105236355A (en) * | 2015-09-25 | 2016-01-13 | 广西大学 | Clean and environmental-protection bleaching powder production process |
| CN109336056A (en) * | 2018-11-20 | 2019-02-15 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of method for preparing calcium hypochlorite by sodium method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1047573C (en) | 1999-12-22 |
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