阅读说明：本技术 一种碱式氯化铜合成中的晶体改性的制备方法 (Preparation method for crystal modification in basic copper chloride synthesis ) 是由 蔡春林 邓志刚 冯一凡 于 2021-08-17 设计创作，主要内容包括：本发明涉及动物饲料生产技术领域,具体公开了一种碱式氯化铜合成中的晶体改性的制备方法,包括如下步骤：室温下,在反应釜中加入氯化铜,然后加入自来水,充分搅拌,直到氯化铜完全溶解；之后加入高分子晶体改进剂至反应釜中,加完后继续搅拌；然后加入氢氧化钠溶液,加完后继续搅拌,然后静置；之后打开反应釜底部转移到真空抽滤装置进行抽滤,得到固体后并用自来水清洗,抽滤完成后,放入干燥箱中恒温干燥；然后取干燥所得产品在恒温恒湿试验箱中进行模拟高温高湿试验。该制备方法工艺简单,操作方便,收率高,没有环境污染,成本低、产品稳定、制备出的产品在高温高湿条件下不容易受潮。(The invention relates to the technical field of animal feed production, and particularly discloses a preparation method for modifying crystals in basic copper chloride synthesis, which comprises the following steps: adding copper chloride into a reaction kettle at room temperature, then adding tap water, and fully stirring until the copper chloride is completely dissolved; then adding a polymer crystal improver into the reaction kettle, and continuing stirring after the addition is finished; then adding sodium hydroxide solution, continuously stirring after adding, and then standing; then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with tap water after obtaining solids, and drying the reaction kettle in a drying oven at constant temperature after filtration is finished; and then taking the dried product to perform a simulated high-temperature high-humidity test in a constant-temperature constant-humidity test box. The preparation method has the advantages of simple process, convenient operation, high yield, no environmental pollution, low cost and stable product, and the prepared product is not easy to be affected with damp under the conditions of high temperature and high humidity.)

1. A preparation method for modifying crystals in basic copper chloride synthesis is characterized by comprising the following steps:

adding copper chloride into a reaction kettle at room temperature, then adding tap water, and fully stirring until the copper chloride is completely dissolved;

then adding a polymer crystal improver into the reaction kettle, and continuing stirring after the addition is finished;

then adding sodium hydroxide solution, continuously stirring after adding, and then standing;

then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with tap water after obtaining solids, and drying the reaction kettle in a drying oven at constant temperature after filtration is finished;

and then taking the dried product to perform a simulated high-temperature high-humidity test in a constant-temperature constant-humidity test box.

2. The method of claim 1, wherein the step of adding industrial solid cupric chloride dihydrate into the reaction kettle, then adding tap water, and fully stirring:

the stirring time is 15-30 minutes.

3. The method of claim 1, wherein the step of adding a polymeric crystal modifier to the reaction vessel is followed by the step of:

the weight ratio of the macromolecular crystal improver is 0.1-1% of the weight of the copper chloride.

4. The method of claim 3, wherein the step of continuing to stir the polymeric crystal modifier after the addition of the polymeric crystal modifier comprises:

the stirring time is 10-20 minutes.

5. The method of claim 4 wherein the modification of the crystals in the synthesis of basic copper chloride is performed,

the polymer crystal improver is calcium lignosulfonate or sodium lignosulfonate.

6. The method of claim 1 wherein the step of adding a sodium hydroxide solution is followed by the step of:

the concentration of the sodium hydroxide solution is 15-40%.

7. The method of claim 1 wherein the step of adding a sodium hydroxide solution is followed by the step of:

the addition time of the sodium hydroxide solution is 20-40 minutes.

8. The method of claim 1, wherein the step of stirring the solution of sodium hydroxide and then allowing the solution to stand is further comprised of:

the continuous stirring time is 20-30 minutes, and the standing time is 30 minutes.

Technical Field

The invention relates to the technical field of animal feed production, in particular to a preparation method for modifying crystals in basic copper chloride synthesis.

Background

The basic copper chloride as the trace element nutrient for animal is a new copper source feed additive which is raised in the twenty-first century, because it has higher bioavailability, does not destroy vitamins and grease in the feed, has very low water solubility, does not corrode production equipment, has uniform grain size, is beneficial to processing, transporting and storing the feed, has high copper content and less required addition amount, and has the characteristics of better biological utilization rate, feed addition safety, feed production economy and the like compared with the traditional feed additive copper sulfate.

The basic copper chloride produced by the process has the advantages of good product stability, difficult moisture and caking and the like compared with the current common basic copper chloride.

However, the process needs heating and mixing different raw materials, and the reaction is complex and difficult to control, so the corresponding production cost is high. If the anti-caking performance of the product can be improved by optimizing the production process of the traditional basic copper chloride, the competitive advantage of the product can be improved.

Disclosure of Invention

The invention aims to provide a preparation method for modifying crystals in basic copper chloride synthesis, and aims to solve the technical problems that different raw materials are required to be heated and then mixed in the production process of basic copper chloride in the prior art, the reaction is complex and difficult to control, and the corresponding production cost is high.

In order to achieve the purpose, the invention adopts a preparation method for modifying crystals in basic copper chloride synthesis, which comprises the following steps:

adding copper chloride into a reaction kettle at room temperature, then adding tap water, and fully stirring until the copper chloride is completely dissolved;

then adding a polymer crystal improver into the reaction kettle, and continuing stirring after the addition is finished;

then adding sodium hydroxide solution, continuously stirring after adding, and then standing;

then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with tap water after obtaining solids, and drying the reaction kettle in a drying oven at constant temperature after filtration is finished;

and then taking the dried product to perform a simulated high-temperature high-humidity test in a constant-temperature constant-humidity test box.

Wherein, add industrial grade solid copper chloride dihydrate in the reation kettle, then add running water, in the step of intensive mixing:

the stirring time is 15-30 minutes.

Wherein, then, adding a polymer crystal modifier into the reaction kettle:

the weight ratio of the macromolecular crystal improver is 0.1-1% of the weight of the copper chloride.

Wherein, the step of continuously stirring after the addition of the polymer crystal improver is as follows:

the stirring time is 10-20 minutes.

Wherein the polymer crystal improver is calcium lignosulfonate or sodium lignosulfonate.

Wherein, in the step of adding the sodium hydroxide solution:

the concentration of the sodium hydroxide solution is 15-40%.

Wherein, in the step of adding the sodium hydroxide solution:

the addition time of the sodium hydroxide solution is 20-40 minutes.

Wherein, after the sodium hydroxide solution is added, the stirring is continued, and then the standing step comprises:

the continuous stirring time is 20-30 minutes, and the standing time is 30 minutes.

The invention relates to a preparation method of crystal modification in basic copper chloride synthesis, which comprises the steps of adding copper chloride into a reaction kettle at room temperature, then adding tap water, and fully stirring until the copper chloride is completely dissolved; then adding a polymer crystal improver into the reaction kettle, and continuing stirring after the addition is finished; then adding sodium hydroxide solution, continuously stirring after adding, and then standing; then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with tap water after obtaining solids, and drying the reaction kettle in a drying oven at constant temperature after filtration is finished; and then taking the dried product to perform a simulated high-temperature high-humidity test in a constant-temperature constant-humidity test box.

The method has the advantages of simple process operation, short synthesis time and no production of ammonia nitrogen compounds, and the final products are the target products of basic copper chloride, sodium chloride and water, so that secondary pollution is avoided; and after the basic copper chloride is crystallized and separated out, a small amount of crystal modifier is adsorbed on the surface of the basic copper chloride, the hydrophobic group faces outwards, and the hydrophilic group faces inwards.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a flow chart of the steps of example 1 of the present invention.

Fig. 2 is a flowchart of the steps of embodiment 2 of the present invention.

Fig. 3 is a flowchart of the steps of embodiment 3 of the present invention.

FIG. 4 is a flowchart of the steps of embodiment 4 of the present invention.

FIG. 5 is a flowchart of the steps of embodiment 5 of the present invention.

Fig. 6 is a flowchart of the steps of embodiment 6 of the present invention.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.

In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

A preparation method for modifying crystals in basic copper chloride synthesis comprises the following steps:

adding copper chloride into a reaction kettle at room temperature, then adding tap water, and fully stirring until the copper chloride is completely dissolved;

then adding a polymer crystal improver into the reaction kettle, and continuing stirring after the addition is finished;

then adding sodium hydroxide solution, continuously stirring after adding, and then standing;

then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with tap water after obtaining solids, and drying the reaction kettle in a drying oven at constant temperature after filtration is finished;

and then taking the dried product to perform a simulated high-temperature high-humidity test in a constant-temperature constant-humidity test box.

Adding industrial-grade solid copper chloride dihydrate into a reaction kettle, then adding tap water, and fully stirring:

the stirring time is 15-30 minutes.

Then adding a polymer crystal modifier into the reaction kettle:

the weight ratio of the macromolecular crystal improver is 0.1-1% of the weight of the copper chloride.

The step of continuing stirring after the addition of the polymer crystal improver is completed:

the stirring time is 10-20 minutes.

The polymer crystal improver is calcium lignosulfonate or sodium lignosulfonate.

Then adding sodium hydroxide solution:

the concentration of the sodium hydroxide solution is 15-40%.

The addition time of the sodium hydroxide solution is 20-40 minutes.

After the sodium hydroxide solution is added, stirring is continued, and then the mixture is stood:

the continuous stirring time is 20-30 minutes, and the standing time is 30 minutes.

Then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, cleaning the reaction kettle with tap water after obtaining solids, and putting the reaction kettle into a drying oven for constant-temperature drying after the filtration is finished:

the water consumption for washing by tap water is 1-500L.

Then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, cleaning the reaction kettle with tap water after obtaining solids, and putting the reaction kettle into a drying oven for constant-temperature drying after the filtration is finished:

the constant temperature drying temperature was 110 ℃.

Then adding sodium hydroxide solution, and in the step of continuing stirring after the sodium hydroxide solution is added, adding copper chloride according to the molar ratio: sodium hydroxide is 2: 3.

in the step of adding copper chloride into the reaction kettle: the concentration of copper chloride is 100-800 g/L.

Example 1, referring to fig. 1, the present invention provides a method for preparing a modified crystal in basic copper chloride synthesis, comprising the following steps:

s1: adding 7.50kg of industrial-grade solid copper chloride dihydrate into a 50L glass reaction kettle at room temperature, adding 10L of tap water, and fully stirring for 15 minutes until the copper chloride is completely dissolved;

s2: then adding 7.5g of crystal modifier sodium lignosulfonate, and continuing stirring for 10 minutes;

s3: then adding 16.6L of 15% sodium hydroxide solution for 20 minutes, continuing stirring for 20 minutes after the addition is finished, and then standing for 30 minutes;

s4: then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with 1L of tap water, and drying the reaction kettle in a drying oven at the constant temperature of 110 ℃ after filtration to obtain 4.4 kg of basic copper chloride powder with the particle size of more than 50 microns;

s5: and then carrying out high-temperature high-humidity simulation comparison experiments on the basic copper chloride.

In the high-temperature and high-humidity simulation comparison experiment of the basic copper chloride: the prepared basic copper chloride sample, the basic copper chloride synthesized without the crystal form improver and products of American micronutries company are simultaneously put into a test box with constant temperature and humidity for experiment, and the result shows that: under the conditions that the temperature of a constant temperature and humidity test box is 50 ℃ and the humidity is 70% RH, the copper chloride hydroxide synthesized by adding the macromolecular crystal improver starts to agglomerate after 30 minutes, the copper chloride hydroxide synthesized by adding the macromolecular crystal improver starts to absorb moisture and agglomerate after 2 hours, and no agglomeration phenomenon is seen in the same treatment time of products of American micronutries company.

Example 2, referring to fig. 2, the present invention provides a method for preparing a modified crystal in basic copper chloride synthesis, comprising the following steps:

s1: adding 7.50kg of industrial-grade solid copper chloride dihydrate into a 50L glass reaction kettle at room temperature, adding 10L of tap water, and fully stirring for 15 minutes until the copper chloride is completely dissolved;

s2: then adding 15g of crystal modifier sodium lignosulfonate, and continuing stirring for 10 minutes;

s3: then adding 9.96L of 25% sodium hydroxide solution for 20 minutes, continuing stirring for 20 minutes after the addition is finished, and then standing for 30 minutes;

s4: then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with 1L of tap water, and drying the reaction kettle in a drying oven at the constant temperature of 110 ℃ after filtration to obtain 4.44 kg of basic copper chloride powder with the particle size of more than 50 microns;

s5: and then carrying out high-temperature high-humidity simulation comparison experiments on the basic copper chloride.

In the high-temperature and high-humidity simulation comparison experiment of the basic copper chloride: the prepared basic copper chloride sample, the basic copper chloride synthesized without the crystal form improver and products of American micronutries company are simultaneously put into a test box with constant temperature and humidity for experiment, and the result shows that: under the conditions that the temperature of a constant temperature and humidity test box is 50 ℃ and the humidity is 70% RH, the product of the copper chloride hydroxide synthesized by adding the crystal improver begins to absorb moisture and agglomerate after 5 hours, and no agglomeration phenomenon is observed in the same time of product treatment of American micronutries company.

Example 3, referring to fig. 3, the present invention provides a method for preparing a modified crystal in basic copper chloride synthesis, comprising the following steps:

s1: adding 7.50kg of industrial-grade solid copper chloride dihydrate into a 50L glass reaction kettle at room temperature, adding 10L of tap water, and fully stirring for 15 minutes until the copper chloride is completely dissolved;

s2: then 22.5g of crystal modifier sodium lignosulfonate is added, and stirring is continued for 10 minutes;

s3: then adding 9.96L of 25% sodium hydroxide solution for 20 minutes, continuing stirring for 20 minutes after the addition is finished, and then standing for 30 minutes;

s4: then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with 1L of tap water, and drying the reaction kettle in a drying oven at the constant temperature of 110 ℃ after filtration to obtain 4.45 kg of basic copper chloride powder with the particle size of more than 50 microns;

s5: and then carrying out high-temperature high-humidity simulation comparison experiments on the basic copper chloride.

In the high-temperature and high-humidity simulation comparison experiment of the basic copper chloride: the prepared basic copper chloride sample, the basic copper chloride synthesized without the crystal form improver and products of American micronutries company are simultaneously put into a test box with constant temperature and humidity for experiment, and the result shows that: under the conditions that the temperature of the constant-temperature constant-humidity test box is 50 ℃ and the humidity is 70% RH, the basic copper chloride synthesized by adding the crystal improver has the moisture absorption and agglomeration phenomenon within 8 hours, and the agglomeration phenomenon is not seen in the same time of product treatment of the American micronutries company.

Example 4, referring to fig. 4, the present invention provides a method for preparing a modified crystal in basic copper chloride synthesis, comprising the following steps:

s1: adding 7.50kg of industrial-grade solid copper chloride dihydrate into a 50L glass reaction kettle at room temperature, adding 10L of tap water, and fully stirring for 15 minutes until the copper chloride is completely dissolved;

s2: then adding 7.5g of crystal modifier calcium lignosulfonate, and continuing stirring for 10 minutes;

s3: then adding 16.6L of 15% sodium hydroxide solution for 20 minutes, continuing stirring for 20 minutes after the addition is finished, and then standing for 30 minutes;

s4: then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with 1L of tap water, and drying the reaction kettle in a drying oven at the constant temperature of 110 ℃ after filtration to obtain 4.42 kg of basic copper chloride powder with the particle size of more than 50 microns;

s5: and then carrying out high-temperature high-humidity simulation comparison experiments on the basic copper chloride.

In the high-temperature and high-humidity simulation comparison experiment of the basic copper chloride: the prepared basic copper chloride sample, the basic copper chloride synthesized without the crystal form improver and products of American micronutries company are simultaneously put into a test box with constant temperature and humidity for experiment, and the result shows that: under the conditions that the temperature of the constant temperature and humidity test box is 50 ℃ and the humidity is 70 percent RH, the basic copper chloride synthesized by adding the crystal improver begins to absorb moisture and agglomerate after 3 hours.

Example 5, referring to fig. 5, the present invention provides a method for preparing a modified crystal in basic copper chloride synthesis, comprising the following steps:

s1: adding 7.50kg of industrial-grade solid copper chloride dihydrate into a 50L glass reaction kettle at room temperature, adding 10L of tap water, and fully stirring for 15 minutes until the copper chloride is completely dissolved;

s2: then adding 15g of crystal modifier calcium lignosulfonate, and continuing stirring for 10 minutes;

s3: then adding 9.96L of 25% sodium hydroxide solution for 20 minutes, continuing stirring for 20 minutes after the addition is finished, and then standing for 30 minutes;

s4: then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with 1L of tap water, and drying the reaction kettle in a drying oven at the constant temperature of 110 ℃ after filtration to obtain 4.46 kg of basic copper chloride powder with the particle size of more than 50 microns;

s5: and then carrying out high-temperature high-humidity simulation comparison experiments on the basic copper chloride.

In the high-temperature and high-humidity simulation comparison experiment of the basic copper chloride: the prepared basic copper chloride sample, the basic copper chloride synthesized without the crystal form improver and products of American micronutries company are simultaneously put into a test box with constant temperature and humidity for experiment, and the result shows that: under the conditions that the temperature of a constant temperature and humidity test box is 50 ℃ and the humidity is 70% RH, the product of the copper chloride hydroxide synthesized by adding the crystal improver begins to absorb moisture and agglomerate after 7 hours, and no agglomeration phenomenon is observed in the same time of product treatment of American micronutries company.

Example 6, referring to fig. 6, the present invention provides a method for preparing a modified crystal in basic copper chloride synthesis, comprising the following steps:

s1: adding 7.50kg of industrial-grade solid copper chloride dihydrate into a 50L glass reaction kettle at room temperature, adding 10L of tap water, and fully stirring for 15 minutes until the copper chloride is completely dissolved;

s2: then adding 15g of crystal modifier calcium lignosulfonate, and continuing stirring for 10 minutes;

s3: then adding 16.6L of 15% sodium hydroxide solution for 20 minutes, continuing stirring for 20 minutes after the addition is finished, and then standing for 30 minutes;

s4: then opening the bottom of the reaction kettle, transferring the reaction kettle to a vacuum filtration device for filtration, washing the reaction kettle with 1L of tap water, and drying the reaction kettle in a drying oven at the constant temperature of 110 ℃ after filtration to obtain 4.48 kg of basic copper chloride powder with the particle size of more than 50 microns;

s5: and then carrying out high-temperature high-humidity simulation comparison experiments on the basic copper chloride.

In the high-temperature and high-humidity simulation comparison experiment of the basic copper chloride: the prepared basic copper chloride sample, the basic copper chloride synthesized without the crystal form improver and products of American micronutries company are simultaneously put into a test box with constant temperature and humidity for experiment, and the result shows that: under the conditions that the temperature of a constant temperature and humidity test box is 50 ℃ and the humidity is 70% RH, the copper chloride hydroxide synthesized by adding the crystal improver has no caking within 48 hours, and the product of American company has slight caking within 35 hours.

In conclusion, the preparation method for modifying the crystal in the synthesis of the basic copper chloride provided by the invention has the advantages of simple process, convenience in operation, high yield, no environmental pollution, low cost, stable product and difficulty in wetting the product under the high-temperature and high-humidity conditions.

While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.