阅读说明：本技术 一种净水剂及其制备方法 (Water purifying agent and preparation method thereof ) 是由 丘关南 蒋志飞 张洪 谭帼英 罗一帜 于 2019-10-12 设计创作，主要内容包括：本发明适用于水处理技术领域,提供了一种净水剂及其制备方法,所述制备方法包括：在搪瓷反应釜加入铝箔酸以及氢氧化铝,并升温至130~160℃,压力控制在0.25~0.35MPa,反应2.5~3.5小时后,制备得到第一聚合双酸铝；将所述第一聚合双酸铝转到玻璃钢常压反应釜,加入水搅拌均匀后,加入铝酸钙粉,聚合反应80~100min后,过滤不溶物,得第二聚合双酸铝；在所述第二聚合双酸铝中加入氯化铁以及六水氯化镁,混合1~2小时,即得。本发明方法工艺简单,所得产品盐基度最高可达95.1%,净化效果更佳,同时减少以往两步法生产中,硫酸根与钙反应生成的硫酸钙结晶物产生,减少二次污染,提高产出率,以及避免产品在客户使用中出现硫酸钙结晶堵塞管道的问题发生。(The invention is suitable for the technical field of water treatment, and provides a water purifying agent and a preparation method thereof, wherein the preparation method comprises the following steps: adding aluminum foil acid and aluminum hydroxide into an enamel reaction kettle, heating to 130-160 ℃, controlling the pressure to be 0.25-0.35 MPa, and reacting for 2.5-3.5 hours to prepare first polymeric aluminum diacetate; transferring the first aluminum polybisilate to a glass fiber reinforced plastic normal-pressure reaction kettle, adding water, uniformly stirring, adding calcium aluminate powder, carrying out polymerization reaction for 80-100 min, and filtering insoluble substances to obtain a second aluminum polybisalate; and adding ferric chloride and magnesium chloride hexahydrate into the second aluminum bis-polymer, and mixing for 1-2 hours to obtain the catalyst. The method has simple process, the basicity of the obtained product can reach 95.1 percent at most, the purification effect is better, the generation of calcium sulfate crystals generated by the reaction of sulfate radicals and calcium in the conventional two-step production is reduced, the secondary pollution is reduced, the yield is improved, and the problem that the pipeline is blocked by the calcium sulfate crystals in the use of the product by customers is avoided.)

1. A preparation method of a water purifying agent is characterized by comprising the following steps:

Weighing the following raw materials in parts by weight: 15-25 parts of aluminum foil acid, 2-6 parts of aluminum hydroxide, 8-12 parts of water, 2-6 parts of calcium aluminate powder, 1-2 parts of ferric chloride and 0.07-0.15 part of magnesium chloride hexahydrate;

adding the aluminum foil acid and the aluminum hydroxide into an enamel reaction kettle, heating to 130-160 ℃, controlling the pressure to be 0.25-0.35 MPa, and reacting for 2.5-3.5 hours to prepare first polymeric aluminum diacetate;

Transferring the first aluminum polybisilate to a glass fiber reinforced plastic normal-pressure reaction kettle, adding water, uniformly stirring, adding calcium aluminate powder, carrying out polymerization reaction for 80-100 min, and filtering insoluble substances to obtain a second aluminum polybisalate;

And adding ferric chloride and magnesium chloride hexahydrate into the second aluminum dimer, starting a circulating pump for circulating stirring, and starting compressed gas for air-floating mixing for 1-2 hours to obtain the catalyst.

2. the method for preparing a water purifying agent according to claim 1, wherein the weight ratio of the aluminum foil acid to the aluminum hydroxide is 5: 1.

3. The method for preparing a water purifying agent according to claim 1, wherein the weight ratio of the ferric chloride to the magnesium chloride hexahydrate is 25: 2.

4. the preparation method of the water purifying agent according to claim 1, wherein the raw materials are weighed according to the following parts by weight: 15-25 parts of aluminum foil acid, 2-6 parts of aluminum hydroxide, 8-12 parts of water, 2-6 parts of calcium aluminate powder, 1-2 parts of ferric chloride and 0.07-0.15 part of magnesium chloride hexahydrate, and comprises the following steps:

weighing the following raw materials in parts by weight: 20 parts of aluminum foil acid, 4 parts of aluminum hydroxide, 10 parts of water, 4 parts of calcium aluminate powder, 1.5 parts of ferric chloride and 0.12 part of magnesium chloride hexahydrate.

5. The method for preparing the water purifying agent according to claim 1, wherein the aluminum foil acid comprises the following components in percentage by weight: 13 to 15 percent of hydrochloric acid, 1.5 to 2.5 percent of sulfuric acid and 30.8 to 1.5 percent of Al2O30.

6. The preparation method of the water purifying agent according to claim 1, wherein the calcium aluminate powder comprises the following components in percentage by weight: 348 to 52 percent of Al2O, 30 to 33 percent of CaO and 1.5 to 2.5 percent of total iron.

7. The method for preparing the water purifying agent according to claim 1, wherein the step of adding the aluminum foil acid and the aluminum hydroxide into an enamel reaction kettle, raising the temperature to 130-160 ℃, controlling the pressure to 0.25-0.35 MPa, and reacting for 2.5-3.5 hours to obtain the first polymeric aluminum bis-carboxylate comprises the following steps:

Adding the aluminum foil acid and the aluminum hydroxide into an enamel reaction kettle, heating to 145 ℃, controlling the pressure to be 0.3MPa, and reacting for 3 hours to obtain the first aluminum bis-polymer.

8. The preparation method of the water purifying agent according to claim 1, wherein the step of transferring the first aluminum polybisilicate to a glass fiber reinforced plastic normal pressure reaction kettle, adding water, stirring uniformly, adding calcium aluminate powder, carrying out polymerization for 80-100 min, and filtering insoluble substances to obtain the second aluminum polybisilicate comprises the following steps:

Transferring the first aluminum polybisilate to a glass fiber reinforced plastic normal-pressure reaction kettle, adding water, uniformly stirring, controlling the temperature to 80-85 ℃, adding calcium aluminate powder, controlling the reaction temperature to 100-110 ℃, carrying out polymerization for 80-100 min, and filtering insoluble substances to obtain the second aluminum polybisilate.

9. The preparation method of the water purifying agent according to claim 1, wherein the step of adding ferric chloride and magnesium chloride hexahydrate into the second polymeric aluminum diacetate, starting a circulating pump for circulating stirring, and starting compressed air for air flotation mixing for 1-2 hours comprises:

And controlling the temperature of the second polymerized aluminum diacid to be 65-70 ℃, adding ferric chloride and magnesium chloride hexahydrate, starting a circulating pump for circulating stirring, and starting compressed air flotation for mixing for 1.5 hours to obtain the product.

10. a water purifying agent, characterized in that the water purifying agent is prepared by the preparation method of the water purifying agent according to any one of claims 1 to 9.

Technical Field

The invention belongs to the technical field of water treatment, and particularly relates to a water purifying agent and a preparation method thereof.

Background

The iron-aluminum copolymerized compound inorganic high molecular water purifying agent is a novel chemical industry researched and developed from seventies to ninety, plays a great role in improving the quality of life of people and treating the environment, and is widely applied to the purification treatment of drinking water, various industrial sewage and the like. .

Wherein, polymeric aluminum ferric sulfate (PFASC) is a nontoxic, safe and high-efficient water purifying agent with strong adsorption and coagulation capacity and better purification effect in the water purification process, however, the PFASC preparation method in the prior art is generally prepared by mixing in one step and normal pressure, and a few PFASC preparations are produced by adopting a two-step method; wherein, the basicity of the product prepared by the one-step normal pressure method is relatively low, and the stability of the purification effect is not good, so that the actual requirements of modern life and industrial water purification can not be met; the two-step method has high cost and complex process, calcium sulfate crystals are very easily generated in the preparation process, secondary pollution is caused, the problem that pipelines are blocked by calcium sulfate crystals in the using process of the product is caused, and the basicity of the obtained product is still low, so that the actual requirements of modern life and industrial purified water cannot be met.

Therefore, the existing PFASC production process generally has the problems of complex process, low basicity, unstable purification effect and easy pipeline blockage.

Disclosure of Invention

The embodiment of the invention provides a preparation method of a water purifying agent, and aims to solve the problems of complex process, low basicity, unstable purifying effect and easy pipeline blockage existing in the conventional PFASC production process.

The embodiment of the invention is realized in such a way that the preparation method of the water purifying agent comprises the following steps:

Weighing the following raw materials in parts by weight: 15-25 parts of aluminum foil acid, 2-6 parts of aluminum hydroxide, 8-12 parts of water, 2-6 parts of calcium aluminate powder, 1-2 parts of ferric chloride and 0.07-0.15 part of magnesium chloride hexahydrate;

Adding the aluminum foil acid and the aluminum hydroxide into an enamel reaction kettle, heating to 130-160 ℃, controlling the pressure to be 0.25-0.35 MPa, and reacting for 2.5-3.5 hours to prepare first polymeric aluminum diacetate;

Transferring the first aluminum polybisilate to a glass fiber reinforced plastic normal-pressure reaction kettle, adding water, uniformly stirring, adding calcium aluminate powder, carrying out polymerization reaction for 80-100 min, and filtering insoluble substances to obtain a second aluminum polybisalate;

And adding ferric chloride and magnesium chloride hexahydrate into the second aluminum dimer, starting a circulating pump for circulating stirring, and starting compressed gas for air-floating mixing for 1-2 hours to obtain the catalyst.

The embodiment of the invention also provides a water purifying agent, which is prepared by the preparation method of the water purifying agent.

In the embodiment of the invention, aluminum foil acid and aluminum hydroxide are utilized to prepare polymeric aluminum sulfate through a two-step method, and FeCl3 solution and magnesium chloride hexahydrate are added as stabilizing agents after specific treatment and filtration to react and polymerize to obtain polymeric aluminum ferric sulfate. On one hand, the method utilizes the aluminum foil acid for production, has low cost and comprehensively utilizes resources; on the other hand, the method has simple process, the basicity of the obtained product can reach 95.1 percent at most, the purification effect is better, the generation of calcium sulfate crystals generated by the reaction of sulfate radicals and calcium in the conventional two-step production is reduced, the secondary pollution is reduced, the yield is improved, and the problem that the pipeline is blocked by the calcium sulfate crystals in the use of the product by customers is avoided.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

According to the preparation method of the water purifying agent provided by the embodiment of the invention, aluminum foil acid and aluminum hydroxide are subjected to specific treatment to prepare polymeric aluminum sulfate with the mass content of Al2O3 being 10.5-11%, FeCl3 solution with the mass content of total iron being 10-13% and magnesium chloride hexahydrate are added after specific treatment and filtration to be used as stabilizers to react and polymerize to obtain polymeric aluminum ferric sulfate, wherein Al + Fe is more than or equal to 10%, and total iron is more than or equal to 1%. On one hand, the method utilizes the aluminum foil acid for production, has low cost and comprehensively utilizes resources; on the other hand, the method has simple process, the basicity of the obtained product can reach 95.1 percent at most, the purification effect is better, the generation of calcium sulfate crystals generated by the reaction of sulfate radicals and calcium in the conventional two-step production is reduced, the secondary pollution is reduced, the yield is improved, and the problem that the pipeline is blocked by the calcium sulfate crystals in the use of the product by customers is avoided.

In an embodiment of the present invention, the preparation method of the water purifying agent includes:

Weighing the following raw materials in parts by weight: 15-25 parts of aluminum foil acid, 2-6 parts of aluminum hydroxide, 8-12 parts of water, 2-6 parts of calcium aluminate powder, 1-2 parts of ferric chloride and 0.07-0.15 part of magnesium chloride hexahydrate;

Adding the aluminum foil acid and the aluminum hydroxide into an enamel reaction kettle, heating to 130-160 ℃, controlling the pressure to be 0.25-0.35 MPa, and reacting for 2.5-3.5 hours to prepare first polymeric aluminum diacetate;

Transferring the first aluminum polybisilate to a glass Fiber Reinforced Plastic (FRP) normal-pressure reaction kettle, adding water, uniformly stirring, adding calcium aluminate powder, carrying out polymerization reaction for 80-100 min, and filtering insoluble substances to obtain a second aluminum polybisalate;

And adding ferric chloride and magnesium chloride hexahydrate into the second aluminum dimer, starting a circulating pump for circulating stirring, and starting compressed gas for air-floating mixing for 1-2 hours to obtain the catalyst.

wherein the aluminum foil acid (Guandong Huafeng New energy science and technology Co., Ltd.), the aluminum hydroxide (Guangxi Pingguo aluminum industry Co., Ltd.), the calcium aluminate powder (Kaili Xintai melt Co., Ltd.), the ferric chloride (Steyr environmental science and technology Co., Ltd.) and the magnesium chloride hexahydrate (Shandong Jiu heavy chemical industry Co., Ltd.) are purchased.

wherein the aluminum foil acid comprises the following components in percentage by weight: 13 to 15 percent of hydrochloric acid, 1.5 to 2.5 percent of sulfuric acid and 30.8 to 1.5 percent of Al2O30.

In the embodiment of the invention, the aluminum foil acid is used for production, and the aluminum foil acid contains 0.8-1.5% of Al2O3, so that the use amounts of aluminum hydroxide and calcium aluminate powder can be reduced, and the product cost is low.

In the embodiment of the invention, the enamel reaction kettle is used for dissolving the aluminum hydroxide at high temperature and high pressure, which is beneficial to improving the dissolution rate of the aluminum hydroxide.

In the embodiment of the invention, the calcium aluminate powder comprises the following components in percentage by weight: 348 to 52 percent of Al2O, 30 to 33 percent of CaO and 1.5 to 2.5 percent of total iron.

In a preferred embodiment of the invention, the raw materials are weighed according to the following parts by weight: 15-25 parts of aluminum foil acid, 2-6 parts of aluminum hydroxide, 8-12 parts of water, 2-6 parts of calcium aluminate powder, 1-2 parts of ferric chloride and 0.07-0.15 part of magnesium chloride hexahydrate, and specifically comprises the following steps:

weighing the following raw materials in parts by weight: 20 parts of aluminum foil acid, 4 parts of aluminum hydroxide, 10 parts of water, 4 parts of calcium aluminate powder, 1.5 parts of ferric chloride and 0.12 part of magnesium chloride hexahydrate.

In a preferred embodiment of the present invention, the step of adding the aluminum foil acid and the aluminum hydroxide into the enamel reactor, heating the mixture to 130 to 160 ℃, controlling the pressure to be 0.25 to 0.35MPa, and reacting the mixture for 2.5 to 3.5 hours to obtain the first polymeric aluminum bis-carboxylate specifically comprises:

Adding the aluminum foil acid and the aluminum hydroxide into an enamel reaction kettle, heating to 145 ℃, controlling the pressure to be 0.3MPa, and reacting for 3 hours to obtain the first aluminum bis-polymer.

In a preferred embodiment of the invention, the weight ratio of the aluminum foil acid to the aluminum hydroxide is preferably 5:1, and researches show that under the specific weight ratio of the aluminum foil acid to the aluminum hydroxide, the polymerized double aluminum sulfate obtained after the polymerization reaction at normal temperature is heated and pressurized has higher basicity, and is beneficial to polymerizing free sulfate radicals into a product, so that calcium sulfate precipitation caused by the reaction with calcium during the subsequent addition of calcium aluminate powder is avoided, insoluble substances are reduced, and the stability of the product is improved.

In a preferred embodiment of the present invention, the step of transferring the first aluminum bis-carboxylate to a glass fiber reinforced plastic normal pressure reaction kettle, adding water, stirring uniformly, adding calcium aluminate powder, performing polymerization for 80-100 min, and filtering insoluble substances to obtain the second aluminum bis-carboxylate specifically comprises:

Transferring the first aluminum polybisilate to a glass fiber reinforced plastic normal-pressure reaction kettle, adding water, uniformly stirring, controlling the temperature to 80-85 ℃, adding calcium aluminate powder, controlling the reaction temperature to 100-110 ℃, carrying out polymerization for 80-100 min, and filtering insoluble substances to obtain the second aluminum polybisilate.

In a preferred embodiment of the present invention, the step of adding ferric chloride and magnesium chloride hexahydrate into the second polymeric aluminum diacid, starting a circulating pump to circularly stir, and starting compressed air to perform air flotation mixing for 1 to 2 hours to obtain the second polymeric aluminum diacid specifically includes:

And controlling the temperature of the second polymerized aluminum diacid to be 65-70 ℃, adding ferric chloride and magnesium chloride hexahydrate, starting a circulating pump for circulating stirring, and starting compressed air flotation for mixing for 1.5 hours to obtain the product.

In a preferred embodiment of the invention, the weight ratio of the ferric chloride to the magnesium chloride hexahydrate is preferably 25:2, and experimental studies show that the obtained polymeric aluminum ferric chloride sulfate product can be stably stored for more than 12 months without deterioration, wherein the insoluble content of the polymeric aluminum ferric sulfate product is less than 0.05% by polymerization reaction with the polymeric aluminum sulfate after a plate-and-frame filter press under the specific weight ratio of the ferric chloride to the magnesium chloride hexahydrate.

The embodiment of the invention also provides a water purifying agent which is a polymeric aluminum ferric sulfate water purifying agent and is prepared by the preparation method of the water purifying agent, the water purifying agent has the performances of aluminum salt, ferric salt, polymeric aluminum chloride and aluminum sulfate, the basicity is larger, and the sewage treatment effect is strong; however, it is worth noting that experimental research shows that the treatment effect of the water purifying agent has obvious correlation with the preparation process parameter conditions.

the method for preparing the water purifying agent and the technical effects of the water purifying agent of the present invention are further described below by specific examples, wherein the content of the non-described components is the weight percentage content.