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Method for preparing fertilizer grade ammonium phosphate concentrated solution by utilizing phosphoric acid-nitric acid-acetic acid waste liquor

A technology for preparing fertilizers and ammonium phosphate, which is applied in the direction of phosphate, phosphorus oxyacids, fertilizer mixtures, etc., can solve the problems of phosphoric acid utilization without further elaboration, interference with plant growth, incompleteness, etc., to achieve resource utilization and process simple effect

Inactive Publication Date: 2012-12-19
SHENZHEN SHENTOU ENVIRONMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patents CN1781842A and CN102167415A introduce a method for incomplete regeneration of waste phosphoric acid: selectively extract and separate waste phosphoric acid with a mixed solution of trialkyl phosphate and aliphatic straight-chain saturated hydrocarbons with 6-13 carbon atoms Acetic acid and nitric acid, and then use alkali metal or alkaline earth metal chloride solution for stripping, the acetic acid and nitric acid in the stripping solution can be used to prepare a new etching solution; but there is no further elaboration on the use of phosphoric acid in the raffinate
On the other hand, acetate ions in waste phosphoric acid are easily degraded by soil microorganisms, and there are few reports about acetate ions interfering with plant growth.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 410 ml of waste phosphoric acid bath solution, that is, waste phosphoric acid A, into a 2-liter glass beaker, add 400 ml of 25% ammonia water under stirring, and the pH value at the end point is 6.6 to obtain 738 ml of ammonium phosphate mixed solution A; the solution is clear and free of mechanical impurities visible to the naked eye , with a slight acetic acid and ammonia odor. Then, the beaker containing 738 milliliters of ammonium phosphate mixed solution A was heated on an electric furnace, evaporated and concentrated to a volume of about 660 to 670 milliliters, and then cooled to room temperature to obtain 626 milliliters of ammonium phosphate concentrated solution A. See Table 1 for the main component contents of waste phosphoric acid A, ammonium phosphate mixed solution A and ammonium phosphate concentrated solution A.

[0037] Table 1 Main components of waste phosphoric acid before and after neutralization in ammonia

[0038]

[0039] A...

Embodiment 2

[0042] First, to simulate the process of mixing waste phosphoric acid bath solution into washing wastewater, take 1000 ml of waste phosphoric acid A and add distilled water to make the volume to 2000 ml to obtain waste phosphoric acid B. Then, 2000 milliliters of waste phosphoric acid B is added in 5 liters of three-necked round-bottomed flasks, the middle mouth is connected with a reflux condenser, the left mouth is connected with an ammonia glass tube, and the right mouth is plugged with a frosted glass stopper; then, feed tap water into the condenser, Open the valve of the liquid ammonia cylinder, pass ammonia gas into the waste phosphoric acid at a rate of 15 liters / minute through the ammonia gas flow meter, and it takes 21 minutes; the pH value at the end of the reaction is 6.5, and a total of 220 grams of ammonia gas is added. After cooling to room temperature, 2110 ml of ammonium phosphate mixture B was obtained. The solution is clear, without visible impurities, and ha...

Embodiment 3

[0047] First, to simulate the process of mixing the waste phosphoric acid tank solution into the washing wastewater, take 200 ml of waste phosphoric acid A and dilute it to 2000 ml with distilled water to obtain waste phosphoric acid C. Then, 2000 milliliters of waste phosphoric acid C was transferred to a 5-liter glass beaker, 177 grams of ammonium bicarbonate was added under stirring, and the end point pH value was 6.1 to obtain 2070 milliliters of ammonium phosphate mixture C; the solution was clear without visible mechanical impurities, Has a slight acetic and ammonia odor. Finally, heat the beaker containing 2070 ml of ammonium phosphate mixture C on an electric furnace, evaporate and concentrate to about 930-940 ml, and then cool to room temperature to obtain 870 ml of ammonium phosphate concentrate C. See Table 3 for the main component contents of waste phosphoric acid C, ammonium phosphate mixed solution C and ammonium phosphate concentrated solution C.

[0048] Table...

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Abstract

The invention relates to a method for preparing a fertilizer grade ammonium phosphate concentrated solution by utilizing phosphoric acid-nitric acid-acetic acid waste liquor discharged in a liquid crystal substrate or semiconductor manufacturing process, belonging to the technical field of industrial waste liquor treatment. The method comprises the following two steps of: (1) respectively directly contacting the phosphoric acid-nitric acid-acetic acid waste liquor containing available phosphorus (P2O5) content of more than 30g / L with alkaline reactants such as ammonia gas, ammonia water or ammonium hydrogen carbonate, and neutralizing until pH value is 6-8; and 2) evaporating and concentrating an alkaline neutralization product to obtain the fertilizer grade ammonium phosphate concentrated solution finished product containing the available phosphorus (P2O5) content of 100-300g / L and nitrogen content of 30-120g / L, wherein the fertilizer grade ammonium phosphate concentrated solution finished product can be taken as a raw material used for producing a compound fertilizer, an organic-inorganic compound fertilizer or a humid-acid-containing liquid fertilizer. The method disclosed by the invention simple in process and is applicable to large-scale centralized processing of waste phosphorous acid, the existing industrial waste liquid is reasonably utilized, and good fertilizer required by the current agricultural production is obtained.

Description

Technical field: [0001] The invention relates to a method for producing fertilizer grade ammonium phosphate concentrate by using phosphoric acid-nitric acid-acetic acid waste liquid, which belongs to the technical field intersecting environmental protection and fertilizer production, especially the technical field of industrial waste liquid. Background technique: [0002] In the aluminum-based electrode etching section in the liquid crystal panel manufacturing process, and the aluminum alloy interconnection wet etching section in the semiconductor manufacturing process, a large amount of phosphoric acid-nitric acid-acetic acid waste solution (hereinafter referred to as "waste phosphoric acid") needs to be discharged. The typical composition ratio of this kind of waste phosphoric acid bath is as follows: phosphoric acid 65-70%, nitric acid 1-3%, acetic acid 3-10%, aluminum ion 0.1-0.3%, water 15-25%. If the waste tank liquid is mixed with washing wastewater, the concentration...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/28C05G1/06C05G3/00
Inventor 王卫红武建刚陈志传胡志刚曾涛
Owner SHENZHEN SHENTOU ENVIRONMENT TECH CO LTD