阅读说明：本技术 一种柠檬酸铵的制备方法 (Preparation method of ammonium citrate ) 是由 崔恒元 于 2020-12-03 设计创作，主要内容包括：本发明公开了一种柠檬酸铵的制备方法,具体涉及柠檬酸铵技术领域,其技术方案是：包括以下制备步骤：S1,先将柠檬酸、水、液氨、防腐剂、阻燃剂、氧化剂、聚醚醚酮、聚氨酯树脂、色母、分散剂、活性剂和促进剂进行购买,购买后,并选出合格的产品；S2,将阻燃剂、聚醚醚酮、聚氨酯树脂、活性剂和促进剂依次分开放入到研磨机中进行研磨,研磨后,将得到的粉体进行分开放置.一种柠檬酸铵的制备方法有益效果是：通过在配比的时候加入合适比例的防腐剂、阻燃剂、聚醚醚酮、聚氨酯树脂、色母和分散剂,从而不仅会提高柠檬酸铵的防腐性能、阻燃性能和耐高低温性能,还会让柠檬酸铵具有多种颜色。(The invention discloses a preparation method of ammonium citrate, in particular to the technical field of ammonium citrate, and the technical scheme is as follows: the preparation method comprises the following preparation steps: s1, purchasing citric acid, water, liquid ammonia, a preservative, a flame retardant, an oxidant, polyether ether ketone, polyurethane resin, color master, a dispersing agent, an active agent and an accelerant, and selecting qualified products after purchasing; s2, sequentially and separately putting the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein the preparation method of the ammonium citrate has the beneficial effects that: by adding the preservative, the flame retardant, the polyether-ether-ketone, the polyurethane resin, the color master batch and the dispersing agent in a proper proportion, the corrosion resistance, the flame retardant performance and the high and low temperature resistance of the ammonium citrate can be improved, and the ammonium citrate can have various colors.)

1. A preparation method of ammonium citrate is characterized by comprising the following steps: the preparation method comprises the following preparation steps:

s1, purchasing 60g-80g of citric acid, 80g-100g of water, 30g-50g of liquid ammonia, 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 4g-6g of color master batch, 2g-4g of dispersing agent, 2g-4g of active agent and 4g-8g of accelerant, and selecting qualified products after purchasing;

s2, sequentially and separately putting 6g-10g of flame retardant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 2g-4g of active agent and 4g-8g of accelerator into a grinding machine for grinding, and separately placing the obtained powder after grinding;

s3, pouring 80g-100g of water and 60g-80g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;

s4, heating the citric acid aqueous solution to 50-80 ℃, and then aminolyzing the citric acid aqueous solution by 30-50 g of liquid ammonia;

s5, putting the solution after ammonolysis into a stirrer with the temperature of 100-110 ℃, and then adding 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone and 8g-12g of polyurethane resin in sequence for stirring for 5-8 min;

s6, cooling the temperature of the stirrer to 80-85 ℃, after cooling, putting 2-4 g of active agent and 4-8 g of accelerant into the stirrer to be stirred for 3-5min, then cooling the temperature of the stirrer to 50-60 ℃, and then putting 4-6 g of color master batch and 2-4 g of dispersing agent into the stirrer to be stirred for 4-6 min;

and S7, taking out the stirred mixture, cooling and crystallizing, drying and drying the mixture after cooling and crystallizing, and putting the mixture into a grinder for grinding to obtain the product.

2. The method of claim 1, wherein the ammonium citrate is prepared by: in S2, after the flame retardant, the polyether ether ketone, the polyurethane resin, the activator, and the accelerator are ground, the grinding machine needs to be cleaned to grind the next material.

3. The method of claim 1, wherein the ammonium citrate is prepared by: and S7, putting the cooled and crystallized mixture into a dryer for drying.

4. The method of claim 1, wherein the ammonium citrate is prepared by: the preservative is made of water-based epoxy resin.

5. The method of claim 1, wherein the ammonium citrate is prepared by: the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 0.5 proportion.

6. The method of claim 1, wherein the ammonium citrate is prepared by: the oxidant is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 1: 1 ratio of the components.

7. The method of claim 1, wherein the ammonium citrate is prepared by: the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.5: 1 ratio of the components.

8. The method of claim 1, wherein the ammonium citrate is prepared by: the active agent is a mixture of diphenyl guanidine and zinc oxide according to the ratio of 1: 1 ratio of the components.

9. The method of claim 1, wherein the ammonium citrate is prepared by: the accelerator is set to accelerator ZDC.

Technical Field

The invention relates to the technical field of ammonium citrate, and particularly relates to a preparation method of ammonium citrate.

Background

Ammonium citrate, also called triammonium citrate, is white deliquescent powder or crystal, is easy to dissolve in water, is decomposed at the melting point and has low toxicity, and is mainly used for chemical analysis, industrial water treatment, metal cleaning, ceramic dispersing agent, permeation aid, detergent raw material and soil conditioner components, and also used in the industries of medicine, electronics and the like, and is used as a chemical reagent in analytical chemistry, such as determination of phosphate in fertilizer, determination of phosphate and effective phosphoric acid in fertilizer, and is used as a cyanide-free electroplating complexing agent in electroplating industry, and is used as an antirust agent in mechanical industry, and is used as a buffering agent, an emulsifying agent and the like in food industry, and is obtained by the action of citric acid and ammonia water.

The prior art has the following defects: when the existing ammonium citrate is used as a rust inhibitor in the mechanical industry, the corrosion resistance, the flame retardant property and the high and low temperature resistance of the existing ammonium citrate are poor, and the color of the existing ammonium citrate is single, so that the service life of the existing ammonium citrate is shortened, and the sales volume of the existing ammonium citrate is reduced.

Therefore, the invention is necessary to develop a preparation method of ammonium citrate.

Disclosure of Invention

Therefore, the invention provides a preparation method of ammonium citrate, which is characterized in that a preservative, a flame retardant, polyether-ether-ketone, polyurethane resin, color master and a dispersing agent are added in a proper proportion during proportioning, so that the corrosion resistance, the flame retardant property and the high and low temperature resistance of the ammonium citrate can be improved, the ammonium citrate can have various colors, and the problems that the existing ammonium citrate is poor in corrosion resistance, flame retardant property and high and low temperature resistance and single in color are solved.

In order to achieve the above purpose, the invention provides the following technical scheme: the preparation method comprises the following preparation steps:

s1, purchasing 60g-80g of citric acid, 80g-100g of water, 30g-50g of liquid ammonia, 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 4g-6g of color master batch, 2g-4g of dispersing agent, 2g-4g of active agent and 4g-8g of accelerant, and selecting qualified products after purchasing;

s2, sequentially and separately putting 6g-10g of flame retardant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 2g-4g of active agent and 4g-8g of accelerator into a grinding machine for grinding, and separately placing the obtained powder after grinding;

s3, pouring 80g-100g of water and 60g-80g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;

s4, heating the citric acid aqueous solution to 50-80 ℃, and then aminolyzing the citric acid aqueous solution by 30-50 g of liquid ammonia;

s5, putting the solution after ammonolysis into a stirrer with the temperature of 100-110 ℃, and then adding 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone and 8g-12g of polyurethane resin in sequence for stirring for 5-8 min;

s6, cooling the temperature of the stirrer to 80-85 ℃, after cooling, putting 2-4 g of active agent and 4-8 g of accelerant into the stirrer to be stirred for 3-5min, then cooling the temperature of the stirrer to 50-60 ℃, and then putting 4-6 g of color master batch and 2-4 g of dispersing agent into the stirrer to be stirred for 4-6 min;

and S7, taking out the stirred mixture, cooling and crystallizing, drying and drying the mixture after cooling and crystallizing, and putting the mixture into a grinder for grinding to obtain the product.

Preferably, in S2, after the flame retardant, the polyether ether ketone, the polyurethane resin, the activator, and the accelerator are ground, the grinding machine needs to be cleaned to grind the next material.

Preferably, in S7, the cooled and crystallized mixture is placed into a dryer for drying.

Preferably, the material of the preservative is water-based epoxy resin.

Preferably, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 0.5 proportion.

Preferably, the oxidizing agent is potassium dichromate and concentrated sulfuric acid according to the ratio of 1: 1 ratio of the components.

Preferably, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.5: 1 ratio of the components.

Preferably, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 1: 1 ratio of the components.

Preferably, the accelerator is provided as accelerator ZDC.

The invention has the beneficial effects that:

according to the invention, citric acid, water and liquid ammonia are selected as main materials, and the preservative with a proper proportion is added in the proportioning process, so that the corrosion resistance of ammonium citrate is greatly improved, the service life of ammonium citrate can be prolonged, then the flame retardant with a proper proportion is added, so that the flame retardant property of ammonium citrate can be effectively improved, the ammonium citrate can not be softened and ignited when used at high temperature, and the polyether-ether-ketone with a proper proportion is added, so that the high and low temperature resistance of ammonium citrate is improved, the corrosion resistance of ammonium citrate is also improved, meanwhile, the polyurethane resin with a proper proportion is added, so that the corrosion resistance of ammonium citrate is improved, the ammonium citrate has the characteristics of high strength, tear resistance and wear resistance, the applicability is improved, and the color master batch and the dispersant with a proper proportion are added, this gives ammonium citrate a variety of colors and thus increases sales.

Detailed Description

The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.

Example 1:

the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:

s1, purchasing 60g-80g of citric acid, 80g-100g of water, 30g-50g of liquid ammonia, 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 4g-6g of color master batch, 2g-4g of dispersing agent, 2g-4g of active agent and 4g-8g of accelerant, and selecting qualified products after purchasing;

s2, sequentially and separately putting 6g-10g of flame retardant, 5g-10g of polyether-ether-ketone, 8g-12g of polyurethane resin, 2g-4g of active agent and 4g-8g of accelerant into a grinding machine for grinding, and separately putting obtained powder after grinding, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerant, the grinding machine needs to be cleaned, so that the next material can be ground;

s3, pouring 80g-100g of water and 60g-80g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;

s4, heating the citric acid aqueous solution to 50-80 ℃, and then aminolyzing the citric acid aqueous solution by 30-50 g of liquid ammonia;

s5, putting the solution after ammonolysis into a stirrer with the temperature of 100-110 ℃, and then adding 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone and 8g-12g of polyurethane resin in sequence for stirring for 5-8 min;

s6, cooling the temperature of the stirrer to 80-85 ℃, after cooling, putting 2-4 g of active agent and 4-8 g of accelerant into the stirrer to be stirred for 3-5min, then cooling the temperature of the stirrer to 50-60 ℃, and then putting 4-6 g of color master batch and 2-4 g of dispersing agent into the stirrer to be stirred for 4-6 min;

and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.

Furthermore, the material of the preservative is aqueous epoxy resin.

Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 0.5 proportion.

Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 1: 1 ratio of the components.

Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.5: 1 ratio of the components.

Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 1: 1 ratio of the components.

Further, the accelerator is provided as accelerator ZDC.

Example 2:

the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:

s1, purchasing 60g of citric acid, 80g of water, 30g of liquid ammonia, 5g of preservative, 6g of flame retardant, 4g of oxidant, 5g of polyether-ether-ketone, 8g of polyurethane resin, 4g of color master batch, 2g of dispersant, 2g of active agent and 4g of accelerant, and selecting qualified products after purchasing;

s2, sequentially and separately putting 6g of flame retardant, 5g of polyether-ether-ketone, 8g of polyurethane resin, 2g of active agent and 4g of accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator, the grinding machine needs to be cleaned, and then the next material can be ground;

s3, pouring 80g of water and 60g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;

s4, heating the citric acid aqueous solution to 50 ℃, and then ammonolyzing the citric acid aqueous solution by 30g of liquid ammonia;

s5, putting the solution after ammonolysis into a stirrer with the temperature of 100 ℃, adding 5g of preservative and 6g of flame retardant, stirring for 3min, adding 4g of oxidant, 5g of polyether-ether-ketone and 8g of polyurethane resin, and stirring for 5 min;

s6, cooling the temperature of the stirrer to 80 ℃, after cooling, putting 2g of the active agent and 4g of the accelerant into the stirrer to be stirred for 3min, then cooling the temperature of the stirrer to 50 ℃, and then putting 4g of the color master batch and 2g of the dispersing agent into the stirrer to be stirred for 4 min;

and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.

Furthermore, the material of the preservative is aqueous epoxy resin.

Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 1 ratio of the components.

Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 1: 0.3 proportion.

Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.4: 1 ratio of the components.

Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 0.5: 1 ratio of the components.

Further, the accelerator is provided as accelerator ZDC.

Example 3:

the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:

s1, purchasing 70g of citric acid, 90g of water, 40g of liquid ammonia, 7.5g of preservative, 8g of flame retardant, 5g of oxidant, 7.5g of polyether-ether-ketone, 10g of polyurethane resin, 5g of color master batch, 3g of dispersing agent, 3g of active agent and 6g of accelerant, and selecting qualified products after purchasing;

s2, sequentially and separately putting 8g of flame retardant, 7.5g of polyether-ether-ketone, 10g of polyurethane resin, 3g of active agent and 6g of accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator, the grinding machine needs to be cleaned, so that the next material can be ground;

s3, pouring 90g of water and 70g of citric acid into a mixer for mixing, thereby obtaining an aqueous citric acid solution;

s4, heating the citric acid aqueous solution to 65 ℃, and then ammonolyzing the citric acid aqueous solution by 40g of liquid ammonia;

s5, putting the solution after ammonolysis into a stirrer with the temperature of 105 ℃, firstly adding 7.5g of preservative, 8g of flame retardant and 5g of oxidant, then stirring for 2min, then adding 7.5g of polyether-ether-ketone and 10g of polyurethane resin, and stirring for 6.5 min;

s6, cooling the temperature of the stirrer to 82.5 ℃, then putting 5g of color master batch and 3g of dispersing agent into the stirrer to be stirred for 3.5min, cooling the temperature of the stirrer to 55 ℃ after cooling, and then putting 3g of active agent and 6g of accelerant into the stirrer to be stirred for 5 min;

and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.

Furthermore, the material of the preservative is aqueous epoxy resin.

Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 0.6: 1 ratio of the components.

Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 0.5: 1 ratio of the components.

Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.7: 1 ratio of the components.

Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 0.6: 1 ratio of the components.

Further, the accelerator is provided as accelerator ZDC.

Example 4:

the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:

s1, purchasing 80g of citric acid, 100g of water, 50g of liquid ammonia, 10g of preservative, 10g of flame retardant, 6g of oxidant, 10g of polyether-ether-ketone, 12g of polyurethane resin, 6g of color master batch, 4g of dispersing agent, 4g of active agent and 8g of accelerant, and selecting qualified products after purchasing;

s2, sequentially and separately putting 10g of flame retardant, 10g of polyether-ether-ketone, 12g of polyurethane resin, 4g of active agent and 8g of accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator, the grinding machine needs to be cleaned, and then the next material can be ground;

s3, pouring 100g of water and 80g of citric acid into a stirrer to mix, thereby obtaining an aqueous citric acid solution;

s4, heating the citric acid aqueous solution to 80 ℃, and then ammonolyzing the citric acid aqueous solution by 50g of liquid ammonia;

s5, putting the solution after ammonolysis into a stirrer at the temperature of 110 ℃, sequentially adding 10g of preservative, 10g of flame retardant, 6g of oxidant and 10g of polyether-ether-ketone, stirring for 6min, adding 12g of polyurethane resin, and stirring for 8 min;

s6, cooling the temperature of the stirrer to 85 ℃, after cooling, putting 4g of active agent and 8g of accelerant into the stirrer to be stirred for 5min, then cooling the temperature of the stirrer to 60 ℃, and then putting 6g of color master batch and 4g of dispersing agent into the stirrer to be stirred for 6 min;

and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.

Furthermore, the material of the preservative is aqueous epoxy resin.

Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 0.8: 1 ratio of the components.

Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 0.7: 1 ratio of the components.

Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 1: 2 in proportion.

Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 3: 1 ratio of the components.

Further, the accelerator is provided as accelerator ZDC.

The ammonium citrates prepared in examples 1 to 4 above were compared to obtain the following data:

as can be seen from the above table, the ammonium citrate prepared in examples 1 to 4 has better performance in terms of corrosion resistance, flame retardancy, high and low temperature resistance, color and life, but the ammonium citrate has different effects in terms of corrosion resistance, flame retardancy, high and low temperature resistance, color and life because the ratio of citric acid to water to liquid ammonia to preservative to flame retardant to oxidant to polyether ether ketone to polyurethane resin to color master batch to dispersant to activator to accelerator is different, wherein: citric acid, water and liquid ammonia are used as main materials, and a proper proportion of preservative is added in the proportioning process, so that the corrosion resistance of the ammonium citrate is greatly improved, the service life of the ammonium citrate can be prolonged, then a proper proportion of flame retardant is added, the flame retardant performance of the ammonium citrate can be effectively improved, the ammonium citrate can not be softened and ignited when used at high temperature, and a proper proportion of polyether-ether-ketone is added, so that the high and low temperature resistance of the ammonium citrate is improved, the corrosion resistance of the ammonium citrate is also improved, meanwhile, a proper proportion of polyurethane resin is added, the corrosion resistance of the ammonium citrate is improved, the ammonium citrate has the characteristics of high strength, tear resistance and wear resistance, the applicability is improved, and the color master batch and the dispersant are added in proper proportion, so that the ammonium citrate has multiple colors, therefore, the sales volume can be increased, after the coating is used, the effect of the embodiment 4 is optimal, various colors are kept while the corrosion resistance, the flame retardant property and the high and low temperature resistance are improved, the service life is prolonged, and the application range is enlarged.

The above description is only a preferred embodiment of the present invention, and any person skilled in the art may modify the present invention or modify it into an equivalent technical solution by using the technical solution described above. Therefore, any simple modifications or equivalent substitutions made in accordance with the technical solution of the present invention are within the scope of the claims of the present invention.