Heavy metal chelating trapping sulfide agent hexasulfoguanidinoformic acid or salt thereof, and preparation method and application thereof

A technology of hexathioguanidine formic acid and hexathioguanidine, which is applied in the field of sulfide heavy metal chelating agent hexathioguanidine formic acid or its salts, can solve the problem of reducing the removal effect of heavy metal ions and sulfide precipitation Small particles, long sedimentation time and other problems, to achieve the effect of not easy secondary pollution, large sedimentation particles, and good treatment effect

Active Publication Date: 2014-02-26
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particles of sulfide precipitates are small, the precipitation time is too long, and it is easy to form colloids, which reduces the removal effect of heavy metal ions, and the sulfide precipitant itself remains in the water, and generates hydrogen sulfide gas when it encounters acid, resulting in secondary pollution.

Method used

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  • Heavy metal chelating trapping sulfide agent hexasulfoguanidinoformic acid or salt thereof, and preparation method and application thereof
  • Heavy metal chelating trapping sulfide agent hexasulfoguanidinoformic acid or salt thereof, and preparation method and application thereof
  • Heavy metal chelating trapping sulfide agent hexasulfoguanidinoformic acid or salt thereof, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Add 2L of water, 790g of potassium hydroxide, and 100g of solid potassium phosphate into the reactor, stir to dissolve, then add 287g of guanidine hydrochloride, the ratio of alkali to guanidine hydrochloride is 4:1, and stir for 15 minutes below 10°C . Then slowly add 540mL carbon disulfide and 500mL acetone mixed solution dropwise, the ratio of the amount of carbon disulfide to guanidine hydrochloride is 3:1, the drop rate is controlled during the dropwise addition, so that the reaction temperature is maintained below 10°C. CS 2 After the dropwise addition was completed, the temperature was raised to 40° C. and the reaction was stirred at a constant temperature for 2 hours. The obtained brown-red liquid was cooled, crystallized and filtered, and the filtrate was extracted with acetone and ethanol respectively, and the final product was dried to constant weight to obtain 792 grams of potassium hexathioguanidinoformate, with a reaction yield of 65.8%.

Embodiment 2

[0063] Add 2L of water, 790g of potassium hydroxide, and 100g of solid potassium phosphate into the reactor, stir to dissolve, then add 287g of guanidine hydrochloride, the ratio of alkali to guanidine hydrochloride is 4:1, and stir for 15 minutes below 10°C . Then slowly add 630mL of carbon disulfide and 500mL of acetone mixed solution dropwise, the ratio of the amount of carbon disulfide to guanidine hydrochloride is 3.5:1, and the drop rate is controlled during the dropwise addition to keep the reaction temperature below 10°C. CS 2 After the dropwise addition was completed, the temperature was raised to 40° C. and the reaction was stirred at a constant temperature for 2 hours. Obtain a brownish-red liquid, cool, crystallize and filter, add 200mL concentrated hydrochloric acid to the filtrate and extract with acetone and ethanol respectively, and finally the product is dried to constant weight to obtain 592 grams of hexathioguanidine formic acid, the reaction yield is 70% ...

Embodiment 3

[0065] Add 2L of water, 790g of potassium hydroxide, and 100g of solid potassium phosphate into the reactor, stir to dissolve, then add 287g of guanidine hydrochloride, the ratio of alkali to guanidine hydrochloride is 4:1, and stir for 15 minutes below 10°C . Then slowly add 720mL of carbon disulfide and 500mL of acetone mixed solution dropwise, the ratio of the amount of carbon disulfide to guanidine hydrochloride is 4:1, and the drop rate is controlled during the dropwise addition to keep the reaction temperature below 10°C. CS 2 After the dropwise addition was completed, the temperature was raised to 40° C. and the reaction was stirred at a constant temperature for 3 hours. The brownish-red liquid was obtained, crystallized by cooling and filtered, and the filtrate was extracted with acetone and ethanol respectively, and the final product was dried to constant weight to obtain 892 grams of potassium hexathioguanidinoformate, with a reaction yield of 74.1%.

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Abstract

The invention discloses a heavy metal chelating trapping sulfide agent, and a preparation method and an application thereof. The heavy metal chelating trapping sulfide agent is hexasulfoguanidinoformic acid having a structure represented by formula I, or a water-soluble salt thereof. The preparation method of the heavy metal chelating trapping sulfide agent comprises the following steps: reacting an aqueous solution of guanidine hydrochloride or guanidine nitrate with an excess amount of an alkali to generate free guanidine, reacting the free guanidine with carbon disulfide under the action of a proper amount of an inorganic phosphate to obtain a heavy metal chelating trapping sulfide agent hexasulfoguanidinoformate, and adding a proper amount of an acid for neutralization to obtain hexasulfoguanidinoformic acid. The heavy metal chelating trapping sulfide agent can be used for removing or trapping heavy metal ions in water, and forms a heavy metal sulfide precipitate having a network structure together with the heavy metal ions in water through a chelating effect, so the relative molecular mass of a chelate is improved, the settling time is shortened, and the stability of the chelate formed by the agent and the heavy metals is increased. The formula I is shown in the specification.

Description

technical field [0001] The invention belongs to the technical field of removing, purifying or trapping heavy metal ions, in particular to a sulfide heavy metal chelating trapping agent hexathioguanidine formic acid or its salt, their preparation method and their application in water treatment . Background technique [0002] Heavy metals refer to metals with a specific gravity greater than or equal to 5.0, such as copper (Cu), lead (Pb), zinc (Zn), tin (Sn), nickel (Ni), cobalt (Co), chromium (Cr), mercury (Hg ), cadmium (Cd), etc., and arsenic (As) is also included in heavy metals because of its chemical properties and environmental behavior are similar to heavy metals. The above-mentioned heavy metal ions exist in the water environment in various physical and chemical forms, and migrate and accumulate in the environment. They have the characteristics of stable properties, high enrichment coefficients, and long toxic and side effects. If not handled properly, excessive hea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/26C02F1/62C02F1/64
Inventor 王风贺郝昊天雷武夏明珠王风云姚宇昂黄澍史均清
Owner NANJING NORMAL UNIVERSITY
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