CN1283554C - Method of manufacturing industrial ammonium aluminium sulfate using waste liquid in production of fosetyl-aluminium bacteriocide - Google Patents
Method of manufacturing industrial ammonium aluminium sulfate using waste liquid in production of fosetyl-aluminium bacteriocide Download PDFInfo
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- CN1283554C CN1283554C CN 200310112658 CN200310112658A CN1283554C CN 1283554 C CN1283554 C CN 1283554C CN 200310112658 CN200310112658 CN 200310112658 CN 200310112658 A CN200310112658 A CN 200310112658A CN 1283554 C CN1283554 C CN 1283554C
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Abstract
The present invention relates to a production method for industrial aluminium ammonium sulfate, specifically to a method of producing industrial ammonium aluminium sulfate by waste liquid in production of ethyl phosphine aluminum bactericide. In the basic method, nitrogen containing waste liquid generated in the process of producing the ethyl phosphine aluminum bactericide is collected, and the molar concentration of contained nitrogen of the waste liquid is measured; then, the molar concentration of nitrogen is regulated into a designated value by a mode of adding water or sulphur ammonium, and the waste liquid is used as mother liquid; according to desired molar ratio of reaction, the prepared mother liquid reacts with aluminum sulfate salt in a reaction kettle; after the complete reaction, materials are cooled for crystallization; and after dehydration, the industrial aluminium ammonium sulfate product is obtained. In the production method, the production waste liquid of the ethyl phosphine aluminum bactericide is used as a raw material to replace the traditional article solid sulfur ammonium for producing the industrial aluminium ammonium sulfate, so the production method can lower the manufacturing cost of the industrial aluminium ammonium sulfate and can lower the processing cost of the production waste liquid of the ethyl phosphine aluminum bactericide simultaneously.
Description
Technical field
The present invention relates to the manufacture method of industrial ammonium aluminium sulfate, specifically is a kind of method with the waste liquid process industry exsiccated ammonium alum in the production of phosethyl Al sterilant.
Background technology
Industrial ammonium aluminium sulfate is mainly used in industries such as papermaking, printing and dyeing, industrial water conditioning.Existing manufacture method mainly is to be raw material with Tai-Ace S 150 with as the solid ammonium sulfate of commodity, and its raw materials cost is higher; On the other hand, in the production process of agricultural chemicals phosethyl Al sterilant, existing manufacturing process can produce a large amount of nitrogenous waste liquids, not only pollutes the environment, and has increased the cost that manufacturing enterprise disposes waste liquid.
Summary of the invention
Technical problem to be solved by this invention is, provide a kind of can be with the production waste liquid of phosethyl Al sterilant as raw material, the method that replaces traditional commodity solid ammonium sulfate to come the process industry exsiccated ammonium alum, make its manufacturing cost that can reduce industrial ammonium aluminium sulfate, can reduce the processing cost that the phosethyl Al sterilant is produced waste liquid simultaneously.
Basic skills of the present invention is that the nitrogenous waste liquid that produces in the production process with the phosethyl Al sterilant is collected, its nitrogenous volumetric molar concentration is measured, by the mode that adds water or add the sulphur ammonium volumetric molar concentration of nitrogen is adjusted into 3～8mol/L then, with it as mother liquor, the mother liquor for preparing is reacted in reactor according to required mol ratio and the aluminum sulfate salt of reaction, after reacting completely material is carried out crystallisation by cooling, dewater again, promptly obtain the industrial ammonium aluminium sulfate product.
On above-mentioned basic skills basis, following several concrete technical scheme can be arranged:
Scheme one is after described nitrogenous waste liquid is measured volumetric molar concentration, is the mother liquor of 3～8mol/L by the mode that adds water or add the sulphur ammonium with its volumetric molar concentration that is mixed with nitrogen; Mother liquor is dropped in the reactor, stir down and drop into solid sulphuric acid aluminium by the required mol ratio gradation of reaction, and be heated to 60～100 ℃, make its whole solubilizing reactions, the back insulated and stirred that reacts completely 0.5～2 hour is put into the crystallizing pond crystallisation by cooling with reacted material and the dehydration back obtains the industrial ammonium aluminium sulfate product.
Scheme two is after described nitrogenous waste liquid is measured volumetric molar concentration, is the mother liquor of 3～8mol/L by the mode that adds water or add the sulphur ammonium with its volumetric molar concentration that is mixed with nitrogen; Earlier alum liquor is dropped in the reactor then, be heated to 70～115 ℃ and stir evaporation, when its when thick, the mol ratio required by reaction drops into mother liquor, after reacting completely, insulated and stirred 0.5～2 hour is put into the crystallizing pond crystallisation by cooling with reacted material and the dehydration back obtains the industrial ammonium aluminium sulfate product.
Scheme three is after described nitrogenous waste liquid is measured volumetric molar concentration, is the mother liquor of 3～8mol/L by the mode that adds water or add the sulphur ammonium with its volumetric molar concentration that is mixed with nitrogen; Get an amount of mother liquor and add reactor, under agitation drop into the metal of a certain amount of aluminium or the hydrate of oxide compound or oxide compound slowly, stir, mol ratio theoretical amount according to sulfuric acid and aluminium or aluminum oxide reaction adds concentrated sulfuric acid solution in reactor, under agitation be incubated 0.5～1 hour, it is reacted completely; Drop in the reactor than with mother liquor according to the required theoretical molar of reaction then, be heated to 60～100 ℃, it is reacted completely, and insulated and stirred is 0.5～2 hour again, and reacted material is put into crystallizing pond crystallisation by cooling and dehydration back acquisition industrial ammonium aluminium sulfate product.
Method technology of the present invention is simple, can make that contained nitrogen participates in the production process of exsiccated ammonium alum in the production waste liquid of phosethyl Al sterilant, greatly reduce the raw materials cost that industrial ammonium aluminium sulfate is produced, the production waste liquid of phosethyl Al sterilant is fully used, has reduced the processing cost that the phosethyl Al sterilant is produced waste liquid.
Embodiment
Embodiment one: the production waste liquid to the phosethyl Al sterilant collected is measured concentration, waste liquid is adjusted into the mother liquor of nitrogenous 4mol/L by the mode that adds water or add the sulphur ammonium; In the 1000L reactor, drop into 250 kilograms mother liquor, add the hydrate solids of 100 kilograms of aluminum oxide again, stir, add 70 kilograms of concentration slowly and be 98% sulfuric acid, be incubated 1 hour, to reaction end; Under agitation add 200 kilograms of above-mentioned mother liquors again, to reacting completely, continue insulation 2 hours, dewater after then material being put into the crystallizing pond crystallisation by cooling, obtain meeting 205 kilograms of the industrial ammonium aluminium sulfate products of national standard.
Embodiment two: the mother liquor that the production waste liquid of phosethyl Al sterilant is adjusted into nitrogenous 4mol/L; In the reactor of 1000L, drop into the alum liquor of 500L, wherein the volumetric molar concentration of aluminium is 0.7mol/L, be heated be evaporated near when thick, agitation condition drops into 300 kilograms of mother liquors down, continue to be stirred to and react completely, be incubated 1.5 hours, dewater after material is put into the crystallizing pond crystallisation by cooling, obtain meeting 340 kilograms of the industrial ammonium aluminium sulfate products of national standard.
Claims (4)
1, a kind of method with the waste liquid process industry exsiccated ammonium alum in the production of phosethyl Al sterilant, it is characterized in that: the nitrogenous waste liquid that produces in the production process with the phosethyl Al sterilant is collected, its nitrogenous volumetric molar concentration is measured, by the mode that adds water or add the sulphur ammonium volumetric molar concentration of nitrogen is adjusted into 3～8mol/L then, with it as mother liquor, the mother liquor for preparing is reacted in reactor according to required mol ratio and the aluminum sulfate salt of reaction, after reacting completely material is carried out crystallisation by cooling, dewater again, obtain the industrial ammonium aluminium sulfate product.
2, the method with the waste liquid process industry exsiccated ammonium alum in the production of phosethyl Al sterilant according to claim 1, it is characterized in that: the volumetric molar concentration that the nitrogenous waste liquid that produces in the production process with the phosethyl Al sterilant is mixed with nitrogen is the mother liquor of 3～8mol/L; Mother liquor is dropped in the reactor, stir down and drop into solid sulphuric acid aluminium by the required mol ratio gradation of reaction, and heat is to 60～100 ℃, make its whole solubilizing reactions, the back insulated and stirred that reacts completely 0.5～2 hour, reacted material is put into crystallizing pond, and crystallisation by cooling and dehydration back obtain the industrial ammonium aluminium sulfate product.
3, the method with the waste liquid process industry exsiccated ammonium alum in the production of phosethyl Al sterilant according to claim 1, it is characterized in that: the volumetric molar concentration that the nitrogenous waste liquid that produces in the production process with the phosethyl Al sterilant is mixed with nitrogen is the mother liquor of 3～8mol/L; Earlier alum liquor is dropped in the reactor then, be heated to 70～115 ℃ and stir evaporation, when its when thick, the mol ratio required by reaction drops into mother liquor, after reacting completely, insulated and stirred 0.5～2 hour is put into crystallizing pond with reacted material, and crystallisation by cooling and dehydration back obtain the industrial ammonium aluminium sulfate product.
4, a kind of method with the waste liquid process industry exsiccated ammonium alum in the production of phosethyl Al sterilant, it is characterized in that: the volumetric molar concentration that the nitrogenous waste liquid that produces in the production process with the phosethyl Al sterilant is mixed with nitrogen is the mother liquor of 3～8mol/L; Get an amount of mother liquor and add reactor, under agitation drop into the hydrate of the oxide compound of the oxide compound of amount of metallic aluminum or aluminium or aluminium slowly, stir, mol ratio theoretical amount according to sulfuric acid and aluminium or aluminum oxide reaction adds concentrated sulfuric acid solution in reactor, under agitation be incubated 0.5～1 hour, it is reacted completely; Drop in the reactor than with mother liquor according to the required theoretical molar of reaction then, be heated to 60～100 ℃, it is reacted completely, and insulated and stirred is 0.5～2 hour again, and reacted material is put into crystallizing pond crystallisation by cooling and dehydration back acquisition industrial ammonium aluminium sulfate product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310112658 CN1283554C (en) | 2003-12-15 | 2003-12-15 | Method of manufacturing industrial ammonium aluminium sulfate using waste liquid in production of fosetyl-aluminium bacteriocide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310112658 CN1283554C (en) | 2003-12-15 | 2003-12-15 | Method of manufacturing industrial ammonium aluminium sulfate using waste liquid in production of fosetyl-aluminium bacteriocide |
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| Publication Number | Publication Date |
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| CN1590300A CN1590300A (en) | 2005-03-09 |
| CN1283554C true CN1283554C (en) | 2006-11-08 |
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| CN 200310112658 Expired - Fee Related CN1283554C (en) | 2003-12-15 | 2003-12-15 | Method of manufacturing industrial ammonium aluminium sulfate using waste liquid in production of fosetyl-aluminium bacteriocide |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103172099B (en) * | 2011-12-21 | 2015-02-18 | 山东国瓷鑫美宇氧化铝有限公司 | Method for producing high purity aluminum ammonium sulfate by using industrial aluminum sulfate and industrial ammonium sulfate |
| CN104926383A (en) * | 2015-06-15 | 2015-09-23 | 句容市绿园农资有限公司 | Method for manufacturing organic fertilizer through waste liquor generated in aliette production |
| CN109650627A (en) * | 2019-01-04 | 2019-04-19 | 南京馥安投资管理有限公司 | A kind of organic liquid waste resource utilization method containing ammonium sulfate |
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Assignee: Jiangsu Lvdun Plant Protection Pesticide Experiment Co., Ltd. Assignor: Zhenjiang Agricultural Science Academy Contract fulfillment period: 2008.10.6 to 2018.10.5 contract change Contract record no.: 2008320001134 Denomination of invention: Method of manufacturing industrial ammonium aluminium sulfate using waste liquid in production of fosetyl-aluminium bacteriocide Granted publication date: 20061108 License type: Exclusive license Record date: 20081212 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.6 TO 2018.10.5; CHANGE OF CONTRACT Name of requester: JIANGSU PROVINCE LVDUNZHIBAO AGRICULTURE CHEMICAL Effective date: 20081212 |
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