Preparation process of efficient nickel boroacylate

Abstract

The invention relates to the technical field of preparation of nickel boroacylate, in particular to a high-efficiency nickel boroacylate preparation process, which comprises the following steps: adding raw materials for preparing nickel boroacylate and a solvent into a reaction kettle; determining the time when basic nickel carbonate dry powder starts to be put and the time when basic nickel carbonate dry powder stops being put; determining whether basic nickel carbonate dry powder feeding parameters are adjusted or not based on a comparison result of a time difference between the basic nickel carbonate dry powder feeding starting moment and the basic nickel carbonate dry powder feeding stopping moment and a preset time difference range; whether stirring is stopped or not is determined based on the material viscosity in the vacuum treatment process; and determining whether to adjust the preparation process parameters of the efficient nickel boroacylate based on the comparison result of the qualified rate of the prepared nickel boroacylate and the preset qualified rate. According to the method, the performance of the nickel boroacylate is improved by improving the control precision of the preparation process of the nickel boroacylate.

Description

Technical Field

[0001] The invention relates to the technical field of nickel borate preparation, and in particular to a high-efficiency nickel borate preparation process. Background Art

[0002] In the direct-addition adhesion promoter for high-strength bonding between rubber and metal, nickel boroacylate plays an important role as a special catalyst. Nickel boroacylate can be used as an effective adhesion promoter, which can not only improve the adhesion between rubber and metal, but also promote the chemical reaction between rubber and metal, and also improve the bonding strength between them, thereby enhancing the adhesion performance. However, the traditional preparation process of high-efficiency nickel boroacylate has some by-products generated due to the inaccurate analysis of the nickel boroacylate preparation process, which reduces the purity of the target product and thus reduces the performance of nickel boroacylate.

[0003] Chinese patent application publication number: CN103849007A discloses an adhesive for rubber / metal composite sealing plates, a preparation method and use thereof, which are characterized in that: the adhesive for rubber / metal composite sealing plates is prepared from nickel sulfate, cobalt sulfate, sodium carbonate, glacial acetic acid, isooctanoic acid and tri-n-butyl borate; the preparation method is: injecting sodium carbonate solution into nickel sulfate / cobalt solution for reaction to obtain nickel carbonate / cobalt; mixing the obtained cobalt carbonate and nickel carbonate to prepare mixed carboxylic acid cobalt nickel; and then performing borylation reaction to obtain borylated cobalt nickel; the purpose is to bond metal rubber composite plates.

[0004] The above technical solution has the problem that the nickel boroacylate preparation process lacks analytical control, resulting in inaccurate control of the nickel boroacylate preparation process and causing the prepared nickel boroacylate to have low adhesion properties. Summary of the invention

[0005] To this end, the present invention provides a highly efficient nickel borate preparation process to overcome the problem in the prior art of lack of analytical control over the nickel borate preparation process, resulting in inaccurate control of the nickel borate preparation process and resulting in low adhesion performance of the prepared nickel borate.

[0006] To achieve the above object, the present invention provides a process for preparing high-efficiency nickel borate, comprising:

[0007] Adding neodecanoic acid, stearic acid and rosin acid into a reaction kettle under a first preset temperature condition, and sealing the reaction kettle and adding a solvent under a second preset temperature condition;

[0008] The time when the basic nickel carbonate dry powder starts to be added is determined based on the average temperature inside the reactor and the degree of dissolution of the raw materials, and the time when the basic nickel carbonate dry powder stops being added is determined based on the pressure increase rate inside the reactor and the number of bubbles generated inside the reactor;

[0009] Determine whether to adjust the basic nickel carbonate dry powder delivery parameters based on the comparison result of the time difference between the start time of delivery of the basic nickel carbonate dry powder and the stop time of delivery of the basic nickel carbonate dry powder and the preset time difference range, wherein the delivery parameters include the delivery speed and the stirring speed of the mixer;

[0010] After determining that the process of adding the basic nickel carbonate dry powder is qualified, the reactor is heated up, and when the average temperature inside the reactor reaches a third preset temperature, constant temperature stirring is performed and propionic acid is added within a preset time. After the propionic acid is added, the temperature is continued to be raised, and when the average temperature inside the reactor reaches a fourth preset temperature, the reactor is vacuum-treated, and whether to stop stirring is determined based on the viscosity of the material during the vacuum treatment process;

[0011] Based on the comparison result of the qualified rate of the prepared nickel borate and the preset qualified rate, it is determined whether to adjust the preparation process parameters of the nickel borate, wherein the preparation process parameters of the high-efficiency nickel borate include a preset time difference range and a preset viscosity.

[0012] Further, determining the time to start adding the basic nickel carbonate dry powder includes:

[0013] The average temperature inside the reactor is compared with the preset temperature range, where

[0014] If the average temperature inside the reactor is not within the preset temperature range, it is determined that no basic nickel carbonate powder is added;

[0015] If the average temperature inside the reactor is within the preset temperature range, the dissolution degree of the prepared raw materials is analyzed to determine the time to start adding the basic nickel carbonate dry powder.

[0016] Further, determining the degree of solubility of the prepared raw materials for analysis includes:

[0017] The solubility of the prepared raw material is compared with the preset solubility, wherein:

[0018] If the solubility of the raw material is less than the preset solubility, it is determined not to add the basic nickel carbonate powder;

[0019] If the solubility of the raw material is greater than or equal to the preset solubility, it is determined to start adding basic nickel carbonate dry powder.

[0020] Further, determining the time to stop adding the basic nickel carbonate dry powder includes:

[0021] The pressure increase rate inside the reactor is compared with the preset pressure increase rate, where:

[0022] If the pressure increase rate inside the reactor is less than the preset increase rate, it is determined to continue adding basic nickel carbonate powder;

[0023] If the pressure increase rate inside the reactor is greater than or equal to the preset increase rate, it is determined to analyze the number of bubbles generated inside the reactor.

[0024] Furthermore, the analysis of the number of bubbles generated inside the reactor includes:

[0025] If the number of bubbles generated inside the reactor is less than the preset number of bubbles, it is determined to continue adding basic nickel carbonate powder;

[0026] If the number of bubbles generated inside the reactor is greater than or equal to the preset number of bubbles, it is determined to stop adding basic nickel carbonate dry powder.

[0027] Further, determining whether to adjust the parameters of the basic nickel carbonate dry powder delivery includes:

[0028] According to the comparison result that the time difference between the start time of adding the basic nickel carbonate dry powder and the stop time of adding the basic nickel carbonate dry powder is not within the preset time difference range, it is determined that the basic nickel carbonate dry powder addition parameters need to be adjusted.

[0029] Further, determining whether to stop stirring includes:

[0030] If the viscosity of the material during the vacuum treatment is greater than or equal to the preset viscosity, the stirring is stopped.

[0031] Furthermore, the viscosity of the material is determined according to the power of the stirrer when the material is stirred during the vacuum treatment process and the density of the material during the vacuum treatment process.

[0032] Further, when determining whether to adjust the parameters of the preparation process of the high-efficiency nickel borate, it includes:

[0033] The qualified rate of the prepared nickel boroacylate is compared with the preset qualified rate, wherein:

[0034] If the qualified rate of the prepared nickel borate is lower than the preset qualified rate, it is determined that the preparation process parameters of the high-efficiency nickel borate need to be adjusted.

[0035] Furthermore, the adjustment amount of the preset solubility degree is negatively correlated with the purity of nickel borate, the adjustment amount of the preset increase rate is negatively correlated with the amount of nickel borate produced, and the adjustment amount of the preset number of bubbles is negatively correlated with the amount of nickel borate produced.

[0036] Compared with the prior art, the beneficial effect of the present invention lies in that the present invention determines whether it is possible to start adding basic nickel carbonate dry powder by analyzing the average temperature inside the reactor and the degree of solubility of the prepared raw materials. Accurate analysis of the temperature and the degree of solubility can help determine the best time to add, avoid incomplete reaction due to early addition or delayed reaction due to late addition, thereby reducing resource waste. By accurately determining the time to start adding basic nickel carbonate dry powder, production efficiency can be improved, time waste in the production process can be reduced, production output and benefits can be increased, and ensuring that basic nickel carbonate dry powder is added under appropriate reaction conditions is conducive to the production of high-quality products, improving product stability and reliability, and meeting product quality standards. By accurately controlling the time of addition, safety hazards caused by improper reaction conditions can be avoided, the safety of the production process can be guaranteed, and the risk of accidents can be reduced.

[0037] Furthermore, the present invention determines whether to stop adding basic nickel carbonate powder by analyzing the pressure increase rate inside the reactor and the number of bubbles generated inside the reactor. By monitoring the pressure increase rate and the number of bubbles, the reaction situation inside the reactor can be discovered in time, excessive addition of basic nickel carbonate powder can be avoided, resource waste can be reduced, and the smooth progress of the reaction process can be ensured. Analysis of the pressure increase rate and the number of bubbles is helpful to control the reaction rate, avoid incomplete reaction or product quality degradation due to too fast or too slow reaction speed, and improve reaction efficiency. Monitoring the pressure and the number of bubbles can help avoid safety risks caused by abnormal conditions generated during the reaction process, ensure the safety and stability of the production process, and stop adding basic nickel carbonate powder in time to avoid product quality degradation due to overreaction or insufficient reaction, which is conducive to the production of efficient nickel borate. Accurate monitoring of the pressure increase rate and the number of bubbles is helpful to determine the best time to stop adding, improve production efficiency, and reduce production time and resource waste.

[0038] Furthermore, the present invention determines whether it is necessary to adjust the basic nickel carbonate dry powder feeding parameters according to the comparison result of the time difference between the time when the basic nickel carbonate dry powder starts to be added and the time when the basic nickel carbonate dry powder stops being added, and the preset time difference range, and when the material agglomeration phenomenon occurs during the process of the basic nickel carbonate dry powder starting to be added and the basic nickel carbonate dry powder stopping being added, it indicates that the basic nickel carbonate dry powder is added too fast or the stirring speed of the mixer is too slow, so that the basic nickel carbonate dry powder in the reactor may be aggregated together to form a lump, resulting in the blockage of the feed port or the internal pipeline of the reactor, affecting the uniform dispersion of the material and the progress of the reaction, thereby causing the time difference between the time when the basic nickel carbonate dry powder starts to be added and the time when the basic nickel carbonate dry powder stops being added. The time difference between the start and stop time of adding the basic nickel carbonate dry powder is too long. At this time, the adding speed of the basic nickel carbonate dry powder is reduced by the first adjustment coefficient and the stirring speed of the mixer is increased by the second adjustment coefficient. When no material agglomeration occurs during the period between the start and stop time of adding the basic nickel carbonate dry powder, it means that the adding speed of the basic nickel carbonate dry powder is too slow, resulting in a long time difference between the start and stop time of adding the basic nickel carbonate dry powder. At this time, the adding speed of the basic nickel carbonate dry powder is increased by the second adjustment coefficient. The above method improves the accuracy of the analysis of the nickel borate preparation process and then improves the accuracy of the control of the nickel borate preparation process to obtain nickel borate with high adhesion properties.

[0039] Furthermore, the present invention compares the actual material viscosity with the preset viscosity to more accurately control the stirring operation during the reaction process. If the material viscosity obviously deviates from the preset value, stopping stirring can avoid excessive or insufficient stirring, thereby ensuring accurate control of the reaction conditions. By stopping stirring in time, uneven reaction or incomplete reaction caused by abnormal material viscosity can be avoided, thereby improving the quality stability of the product. Avoiding unnecessary stirring operations can reduce energy consumption, reduce production costs, and improve production efficiency. Stopping stirring at an appropriate time can reduce the load on the equipment, extend the service life of the equipment, and reduce the cost of equipment maintenance and replacement. By accurately controlling the stirring operation, the stability and consistency of the production process can be improved, thereby improving production efficiency.

[0040] Furthermore, the present invention determines whether it is necessary to adjust the parameters of the preparation process of the high-efficiency nickel borate according to the comparison result of the qualified rate of the prepared nickel borate with the preset qualified rate, and when it is determined that the parameters of the preparation process of the high-efficiency nickel borate need to be adjusted, the effectiveness of the adjustment process of the parameters of the basic nickel carbonate dry powder is determined according to the comparison result of the proportion of the adjustment of the basic nickel carbonate dry powder feeding parameters in the preparation process of unqualified high-efficiency nickel borate with the preset proportion. When the proportion is greater than or equal to the preset proportion, it means that the adjustment process of the basic nickel carbonate dry powder feeding parameters is not thorough enough. At this time, the third adjustment coefficient is used to reduce the preset time difference range and thereby increase the adjustment intensity of the adjustment process of the basic nickel carbonate dry powder feeding parameters. When the proportion is less than the preset proportion, it means that the adjustment process of the basic nickel carbonate dry powder feeding parameters is effective. At this time, the fourth adjustment coefficient is used to reduce the viscosity of the material and thereby improve the qualification of the material. The above method improves the accuracy of the analysis of the nickel borate preparation process and thereby improves the accuracy of the control of the nickel borate preparation process to obtain nickel borate with high adhesion performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 The flowchart of the preparation process of efficient nickel boroacylate according to the embodiment of the present invention;

[0042] Figure 2 A flowchart for determining whether to stop stirring in the preparation process of efficient nickel boroacylate according to an embodiment of the present invention;

[0043] Figure 3 The present invention provides a flowchart for determining whether to adjust the parameters of the preparation process of efficient nickel boroacylate according to the preparation process of efficient nickel boroacylate in an embodiment of the present invention. DETAILED DESCRIPTION

[0044] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0045] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0046] It should be noted that, in the description of the present invention, terms such as "up", "down", "left", "right", "inside" and "outside" indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings. This is merely for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention.

[0047] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0048] See also Figure 1-Figure 3 As shown, Figure 1 The flowchart of the preparation process of efficient nickel boroacylate according to the embodiment of the present invention; Figure 2 A flowchart for determining whether to stop stirring in the preparation process of efficient nickel boroacylate according to an embodiment of the present invention; Figure 3 The present invention provides a flowchart for determining whether to adjust the parameters of the preparation process of efficient nickel boroacylate according to the preparation process of efficient nickel boroacylate in an embodiment of the present invention.

[0049] The preparation process of the highly efficient nickel boroacylate of the embodiment of the present invention comprises:

[0050] Step S1, adding neodecanoic acid, stearic acid and rosin acid into a reaction kettle under a first preset temperature condition, and sealing the reaction kettle and adding a solvent under a second preset temperature condition;

[0051] Step S2, determining the time to start adding the basic nickel carbonate powder based on the average temperature inside the reactor and the degree of solubility of the raw materials, and determining the time to stop adding the basic nickel carbonate powder based on the pressure increase rate inside the reactor and the number of bubbles generated inside the reactor;

[0052] Step S3, determining whether to adjust the basic nickel carbonate dry powder delivery parameters based on the comparison result of the time difference between the start time of delivery of the basic nickel carbonate dry powder and the stop time of delivery of the basic nickel carbonate dry powder and a preset time difference range, wherein the delivery parameters include delivery speed and stirring speed of the mixer;

[0053] Step S4, after determining that the process of adding the basic nickel carbonate dry powder is qualified, the reactor is heated up, and when the average temperature inside the reactor reaches a third preset temperature, constant temperature stirring is performed and propionic acid is added within a preset time, and the temperature is continued to be raised after the propionic acid is added, and when the average temperature inside the reactor reaches a fourth preset temperature, the reactor is vacuum-treated, and whether to stop stirring is determined based on the viscosity of the material during the vacuum treatment process;

[0054] Step S5, determining whether to adjust the preparation process parameters of nickel borylate based on the comparison result between the qualified rate of the prepared nickel borylate and the preset qualified rate, wherein the preparation process parameters of the high-efficiency nickel borylate include a preset time difference range and a preset viscosity.

[0055] In the embodiment of the present invention, the first preset temperature condition is not higher than 150°C, the second preset temperature condition is not higher than 133°C, the raw materials for preparing the nickel boroacylate include but are not limited to "neodecanoic acid, stearic acid, rosin acid and propionic acid", and the solvent is preferably an environmentally friendly solvent oil.

[0056] Specifically, in step S2, when determining the time to start adding the basic nickel carbonate dry powder, the addition of the basic nickel carbonate dry powder is determined based on the comparison result that the average temperature inside the reactor is within the preset temperature range, or the degree of solubility of the prepared raw materials is analyzed based on the comparison result that the average temperature inside the reactor is not within the preset temperature range.

[0057] The value range of the preset temperature range in the embodiment of the present invention is set to 85° C.-90° C., but the above value is not limited thereto, and those skilled in the art can also adjust the value according to actual needs.

[0058] In the embodiment of the present invention, when the reactor is heated until the basic nickel carbonate dry powder is added, the furnace temperature is set to 150° C. to heat the reactor.

[0059] Specifically, in step S2, when determining to analyze the solubility of the raw material, it is determined whether to add basic nickel carbonate powder according to the comparison result of the solubility of the raw material and the preset solubility;

[0060] When the degree of dissolution is less than the preset degree of dissolution, it is determined that no basic nickel carbonate dry powder is added;

[0061] When the degree of dissolution is greater than or equal to the preset degree of dissolution, it is determined to start adding basic nickel carbonate dry powder.

[0062] The solubility degree described in the embodiment of the present invention can be characterized by measuring the concentration of the solute in the solution, including being achieved by various chemical analysis methods, such as a spectrophotometer and chromatography. The value of the preset solubility degree is the historical average value of the concentration of the solute in the solution when the solution is free of suspension and precipitation, but the above value is not limited to this, and technicians in this field can also adjust the value according to actual needs.

[0063] In the embodiment of the present invention, the feeding process of the basic nickel carbonate dry powder is maintained at a uniform speed. The uniform feeding can be achieved by conveying the material to the reactor through a screw conveyor, while the flow rate of the material is monitored in real time by a sensor, and the speed of the screw conveyor is automatically adjusted according to the set flow value.

[0064] The present invention determines whether to start adding basic nickel carbonate dry powder by analyzing the average temperature inside the reactor and the degree of solubility of the raw materials for preparation. Accurate analysis of the temperature and the degree of solubility can help determine the best time to add, avoid incomplete reaction due to too early addition or delayed reaction due to too late addition, thereby reducing resource waste. By accurately determining the time to start adding basic nickel carbonate dry powder, production efficiency can be improved, time waste in the production process can be reduced, production output and benefits can be increased, and ensuring that basic nickel carbonate dry powder is added under appropriate reaction conditions is conducive to the production of high-quality products, improves product stability and reliability, and meets product quality standards. By accurately controlling the time of addition, safety hazards caused by improper reaction conditions can be avoided, the safety of the production process is guaranteed, and the risk of accidents is reduced.

[0065] Specifically, in step S2, when it is determined that the time to stop adding the basic nickel carbonate powder is determined, whether to continue adding the basic nickel carbonate powder is determined according to the comparison result of the pressure increase rate inside the reactor and the preset pressure increase rate;

[0066] When the pressure increase rate inside the reactor is lower than the preset increase rate, it is determined to continue adding basic nickel carbonate dry powder;

[0067] When the pressure increase rate inside the reactor is higher than or equal to the preset increase rate, determining the number of bubbles generated inside the reactor;

[0068] Among them, the preset value of the increase rate is the historical average value of the pressure increase rate inside the reactor when signs of pot swelling appear, but the above value is not limited to this, and technical personnel in this field can also adjust the value according to actual needs.

[0069] Specifically, in step S2, when determining the analysis of the number of bubbles generated inside the reactor, it is determined whether to continue to add basic nickel carbonate dry powder according to the comparison result of the number of bubbles generated inside the reactor and the preset number of bubbles;

[0070] When the number of bubbles generated inside the reactor is less than the preset number of bubbles, it is determined to continue adding basic nickel carbonate dry powder;

[0071] When the number of bubbles generated in the reactor is greater than or equal to the preset number of bubbles, it is determined to stop adding basic nickel carbonate dry powder;

[0072] Among them, the preset value of the number of bubbles is the historical average value of the number of bubbles generated inside the reactor when signs of pot swelling appear, but the above value is not limited to this, and technical personnel in this field can also adjust the value according to actual needs.

[0073] The signs of pot swelling described in the embodiments of the present invention include but are not limited to "sudden generation of bubbles or gas emissions accompanied by abnormal reaction sounds, generation of thick smoke or release of harmful gases, and solution overflowing the edge of the container."

[0074] The present invention determines whether to stop adding basic nickel carbonate dry powder by analyzing the pressure increase rate inside the reactor and the number of bubbles generated inside the reactor. By monitoring the pressure increase rate and the number of bubbles, the reaction situation inside the reactor can be discovered in time, and excessive addition of basic nickel carbonate dry powder can be avoided, resource waste can be reduced, and the smooth progress of the reaction process can be ensured. Analysis of the pressure increase rate and the number of bubbles is helpful to control the reaction rate, and incomplete reaction or product quality degradation caused by too fast or too slow reaction speed can be avoided, and the reaction efficiency can be improved. Monitoring the pressure and the number of bubbles can help avoid safety risks caused by abnormal conditions generated during the reaction process, and ensure the safety and stability of the production process. By stopping the addition of basic nickel carbonate dry powder in time, overreaction or insufficient reaction can be avoided to cause product quality degradation, which is conducive to the production of efficient nickel borate. Accurate monitoring of the pressure increase rate and the number of bubbles is helpful to determine the best time to stop adding, and the production efficiency is improved, and the production time and resource waste are reduced.

[0075] Specifically, in step S3, when determining whether to adjust the basic nickel carbonate dry powder delivery parameters, it is determined whether the basic nickel carbonate dry powder delivery parameters need to be adjusted based on the comparison result of the time difference between the start time of the basic nickel carbonate dry powder delivery and the stop time of the basic nickel carbonate dry powder delivery and the preset time difference range;

[0076] When the time difference between the start time of adding the basic nickel carbonate dry powder and the stop time of adding the basic nickel carbonate dry powder does not exceed the preset time difference range, it is determined that there is no need to adjust the basic nickel carbonate dry powder feeding parameters;

[0077] When the time difference between the start time of adding the basic nickel carbonate dry powder and the stop time of adding the basic nickel carbonate dry powder exceeds the preset time difference range, it is determined that the basic nickel carbonate dry powder addition parameters need to be adjusted;

[0078] Among them, the minimum value of the preset time difference range is preferably four-fifths of the historical average time difference between the start time and the stop time of adding the basic nickel carbonate dry powder, and the maximum value of the preset time difference range is preferably six-fifths of the historical average time difference between the start time and the stop time of adding the basic nickel carbonate dry powder, but the above values ​​are not limited to this, and technical personnel in this field can also adjust the value according to actual needs.

[0079] The basic nickel carbonate dry powder delivery parameters described in the embodiment of the present invention include delivery speed and stirring speed of the mixer.

[0080] Specifically, when it is determined that the feeding parameters of basic nickel carbonate dry powder need to be adjusted, the feeding speed is adjusted by the first adjustment coefficient and the stirring speed of the mixer is adjusted by the second adjustment coefficient based on the occurrence of material agglomeration during the period between the start time of feeding the basic nickel carbonate dry powder and the stop time of feeding the basic nickel carbonate dry powder, or the feeding speed is adjusted by the second adjustment coefficient based on the absence of material agglomeration during the period between the start time of feeding the basic nickel carbonate dry powder and the stop time of feeding the basic nickel carbonate dry powder.

[0081] In the embodiment of the present invention, the value range of the first adjustment coefficient is set to 0.82-0.97, and the value range of the second adjustment coefficient is set to 1.05-1.2.

[0082] The present invention determines whether it is necessary to adjust the basic nickel carbonate dry powder feeding parameters according to the comparison result of the time difference between the time when the basic nickel carbonate dry powder starts to be added and the time when the basic nickel carbonate dry powder stops being added and the preset time difference range, and when the material agglomeration phenomenon occurs during the process of the basic nickel carbonate dry powder starting to be added and the basic nickel carbonate dry powder stopping being added, it indicates that the basic nickel carbonate dry powder is added too fast or the stirring speed of the mixer is too slow, so that the basic nickel carbonate dry powder in the reactor may be aggregated together to form a block, resulting in blocking the feeding port or the internal pipeline of the reactor, affecting the uniform dispersion of the material and the progress of the reaction, thereby causing the basic nickel carbonate dry powder to start to be added and the basic nickel carbonate dry powder to stop being added. The time difference between the two moments is too long. At this time, the first adjustment coefficient is used to reduce the feeding speed of the basic nickel carbonate powder and the second adjustment coefficient is used to increase the stirring speed of the mixer. When no material agglomeration occurs during the time when the basic nickel carbonate powder starts to be fed and the time when the basic nickel carbonate powder stops being fed, it means that the feeding speed of the basic nickel carbonate powder is too slow, resulting in a long time difference between the time when the basic nickel carbonate powder starts to be fed and the time when the basic nickel carbonate powder stops being fed. At this time, the feeding speed of the basic nickel carbonate powder is increased by the second adjustment coefficient. The above method improves the accuracy of the analysis of the nickel borate preparation process and then improves the accuracy of the control of the nickel borate preparation process to obtain nickel borate with high adhesion properties.

[0083] Specifically, in step S4, when determining whether to stop stirring, it is determined whether to stop stirring according to the comparison result between the viscosity of the material during the vacuum treatment process and the preset viscosity;

[0084] When the viscosity of the material during the vacuum treatment process is greater than or equal to the preset viscosity, the stirring is stopped;

[0085] When the viscosity of the material during the vacuum treatment is less than the preset viscosity, it is determined to continue stirring;

[0086] The preset viscosity has a value range of 0.7-1, and the preset viscosity is preferably 0.92, but the value is not limited thereto, and those skilled in the art may also adjust the value according to actual needs.

[0087] The viscosity of the material during the vacuum treatment process in the embodiment of the present invention is calculated based on the power of the stirrer when stirring the material during the vacuum treatment process and the density of the material during the vacuum treatment process. The power of the stirrer when stirring the material during the vacuum treatment process and the density of the material during the vacuum treatment process are positively correlated with the viscosity of the material during the vacuum treatment process.

[0088] In the embodiment of the present invention, when it is determined to stop stirring, the material needs to be taken out in time.

[0089] The present invention compares the actual material viscosity with the preset viscosity, and can more accurately control the stirring operation during the reaction process. If the material viscosity obviously deviates from the preset value, stopping stirring can avoid excessive or insufficient stirring, thereby ensuring accurate control of the reaction conditions. By stopping stirring in time, uneven reaction or incomplete reaction caused by abnormal material viscosity can be avoided, thereby improving the quality stability of the product. Avoiding unnecessary stirring operations can reduce energy consumption, reduce production costs, and improve production efficiency. Stopping stirring at an appropriate time can reduce the load on the equipment, extend the service life of the equipment, and reduce the cost of equipment maintenance and replacement. By accurately controlling the stirring operation, the stability and consistency of the production process can be improved, thereby improving production efficiency.

[0090] Specifically, in step S5, when determining whether to adjust the preparation process parameters of the high-efficiency nickel borate, it is determined that there is no need to adjust the preparation process parameters of the high-efficiency nickel borate based on the comparison result that the qualified rate of the prepared nickel borate is greater than or equal to the preset qualified rate, or it is determined that there is a need to adjust the preparation process parameters of the high-efficiency nickel borate based on the comparison result that the qualified rate of the prepared nickel borate is less than the preset qualified rate.

[0091] In the embodiment of the present invention, the value range of the preset qualified rate is set to 0.8-1, and the value of the preset qualified rate is preferably 0.88, but the above value is not limited thereto, and those skilled in the art may also adjust the value according to actual needs.

[0092] The determination of whether the prepared nickel boroacylate is qualified in the embodiment of the present invention includes that the prepared nickel boroacylate is yellow-green particles, the nickel content is 20.5%-21.5%, the heptane insoluble matter is ≤2%, the heating loss % is ≤1% and contains qualitative boron.

[0093] Specifically, in step S5, when it is determined that the parameters of the preparation process of the high-efficiency nickel borate are required to be adjusted, the adjustment method is determined according to the comparison result of the proportion of the adjustment of the basic nickel carbonate dry powder feeding parameters in the preparation process of the unqualified high-efficiency nickel borate and the preset proportion;

[0094] When the proportion of adjustment of the basic nickel carbonate dry powder feeding parameters in the unqualified high-efficiency nickel borate preparation process is greater than or equal to the preset proportion, it is determined to adjust the preset time difference range by the third adjustment coefficient;

[0095] When the proportion of adjustment of the basic nickel carbonate dry powder feeding parameters in the preparation process of unqualified high-efficiency nickel borate, is less than the preset proportion, it is determined to adjust the preset viscosity by the fourth adjustment coefficient;

[0096] In the embodiment of the present invention, the value range of the preset ratio is set to 0.7-1, and the value of the preset ratio is preferably 0.86, but the above value is not limited thereto, and those skilled in the art may also adjust the value according to actual needs.

[0097] In the embodiment of the present invention, the value range of the third adjustment coefficient is set to 0.81-0.96, and the value range of the fourth adjustment coefficient is set to 0.79-0.95.

[0098] The present invention determines whether it is necessary to adjust the parameters of the preparation process of the high-efficiency nickel borate according to the comparison result of the qualified rate of the prepared nickel borate with the preset qualified rate, and when it is determined that the parameters of the preparation process of the high-efficiency nickel borate need to be adjusted, the effectiveness of the adjustment process of the parameters of the basic nickel carbonate dry powder is determined according to the comparison result of the proportion of the adjustment of the basic nickel carbonate dry powder feeding parameters in the preparation process of unqualified high-efficiency nickel borate and the preset proportion. When the proportion is greater than or equal to the preset proportion, it means that the adjustment process of the basic nickel carbonate dry powder feeding parameters is not thorough enough. At this time, the preset time difference range is reduced by the third adjustment coefficient to thereby improve the adjustment strength of the adjustment process of the basic nickel carbonate dry powder feeding parameters. When the proportion is less than the preset proportion, it means that the adjustment process of the basic nickel carbonate dry powder feeding parameters is effective. At this time, the fourth adjustment coefficient is used to reduce the viscosity of the material to thereby improve the qualification of the material. The above method improves the accuracy of the analysis of the nickel borate preparation process and thereby improves the accuracy of the control of the nickel borate preparation process to obtain nickel borate with high adhesion performance.

[0099] Example 1: The present invention selects cobalt boroacylate, nickel boroacylate prepared by the present invention and nickel boroacylate prepared by a general method to conduct three groups of experiments on initial steel wire extraction force, 48h steel wire extraction force and 72h steel wire extraction force, and the experimental data are shown in the following table:

[0100]

[0101] From the data in the table of Example 1, it can be concluded that the nickel boroacylate prepared by the present invention requires greater force in the experiments of initial steel wire extraction force, 48h heat-aged steel wire extraction force and 72h heat-aged steel wire extraction force than cobalt boroacylate and other nickel boroacylate prepared by general methods. Therefore, the adhesion performance of the nickel boroacylate prepared by the present invention is better than that of cobalt boroacylate and other nickel boroacylate prepared by general methods.

[0102] Example 2: Three groups of nickel boroacylate prepared by the method of the present invention in the laboratory and three groups of nickel boroacylate prepared by the general method in the laboratory were selected as experimental groups, and the preparation time and the amount of basic nickel carbonate dry powder used were recorded respectively. The experimental data are shown in the following table:

[0103]

[0104]

[0105] It can be seen from the data recorded in the table of Example 2 that the nickel boroacylate prepared by the method of the present invention not only has a shorter preparation time than the nickel boroacylate prepared by the general method, but also the use amount of the basic nickel carbonate dry powder is more accurate than that in the preparation process of the general method because the present invention accurately determines the start time and the stop time of adding the basic nickel carbonate dry powder during the preparation process, thereby avoiding waste. Therefore, the present invention achieves the purpose of efficiently preparing nickel boroacylate.

[0106] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

[0107] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A process for preparing highly efficient nickel boroacylate, characterized in that: include: Adding neodecanoic acid, stearic acid and rosin acid into a reaction kettle under a first preset temperature condition, and sealing the reaction kettle and adding a solvent under a second preset temperature condition; The time when the basic nickel carbonate powder starts to be added is determined based on the average temperature inside the reactor and the degree of dissolution of the raw materials, and the time when the basic nickel carbonate powder stops being added is determined based on the pressure increase rate inside the reactor and the number of bubbles generated inside the reactor; Determine whether to adjust the basic nickel carbonate dry powder delivery parameters based on the comparison result of the time difference between the start time of delivery of the basic nickel carbonate dry powder and the stop time of delivery of the basic nickel carbonate dry powder and the preset time difference range, wherein the delivery parameters include the delivery speed and the stirring speed of the mixer; After determining that the process of adding the basic nickel carbonate dry powder is qualified, the reactor is heated up, and when the average temperature inside the reactor reaches a third preset temperature, constant temperature stirring is performed and propionic acid is added within a preset time. After the propionic acid is added, the temperature is continued to be raised, and when the average temperature inside the reactor reaches a fourth preset temperature, the reactor is vacuum-treated, and whether to stop stirring is determined based on the viscosity of the material during the vacuum treatment process; Based on the comparison result of the qualified rate of the prepared nickel borate and the preset qualified rate, it is determined whether to adjust the preparation process parameters of the nickel borate, wherein the preparation process parameters of the high-efficiency nickel borate include a preset time difference range and a preset viscosity.

2. The process for preparing high-efficiency nickel boroacylate according to claim 1, characterized in that: Determining the time to start adding basic nickel carbonate powder includes: The average temperature inside the reactor is compared with the preset temperature range, where If the average temperature inside the reactor is not within the preset temperature range, it is determined that no basic nickel carbonate powder is added; If the average temperature inside the reactor is within the preset temperature range, the dissolution degree of the prepared raw materials is analyzed to determine the time to start adding the basic nickel carbonate dry powder.

3. The process for preparing high-efficiency nickel boroacylate according to claim 2, characterized in that: Analyses to determine the solubility of the prepared raw materials include: The solubility of the prepared raw material is compared with the preset solubility, wherein: If the solubility of the raw material is less than the preset solubility, it is determined not to add the basic nickel carbonate powder; If the solubility of the raw material is greater than or equal to the preset solubility, it is determined to start adding basic nickel carbonate dry powder.

4. The process for preparing high-efficiency nickel boroacylate according to claim 3, characterized in that: Determining the time to stop adding basic nickel carbonate powder includes: The pressure increase rate inside the reactor is compared with the preset pressure increase rate, where: If the pressure increase rate inside the reactor is less than the preset increase rate, it is determined to continue adding basic nickel carbonate powder; If the pressure increase rate inside the reactor is greater than or equal to the preset increase rate, it is determined to analyze the number of bubbles generated inside the reactor.

5. The process for preparing high-efficiency nickel boroacylate according to claim 4, characterized in that: Analysis of the number of bubbles generated inside the reactor includes: If the number of bubbles generated inside the reactor is less than the preset number of bubbles, it is determined to continue adding basic nickel carbonate powder; If the number of bubbles generated inside the reactor is greater than or equal to the preset number of bubbles, it is determined to stop adding basic nickel carbonate dry powder.

6. The process for preparing high-efficiency nickel boroacylate according to claim 5, characterized in that: Determine whether to adjust the parameters of basic nickel carbonate dry powder, including: According to the comparison result that the time difference between the start time of adding the basic nickel carbonate dry powder and the stop time of adding the basic nickel carbonate dry powder is not within the preset time difference range, it is determined that the basic nickel carbonate dry powder addition parameters need to be adjusted.

7. The process for preparing high-efficiency nickel boroacylate according to claim 6, characterized in that: Determining whether to stop stirring includes: If the viscosity of the material during the vacuum treatment is greater than or equal to the preset viscosity, the stirring is stopped.

8. The process for preparing high-efficiency nickel boroacylate according to claim 7, characterized in that: The viscosity of the material is determined according to the power of the stirrer when the material is stirred during the vacuum treatment process and the density of the material during the vacuum treatment process.

9. The process for preparing high-efficiency nickel boroacylate according to claim 8, characterized in that: When determining whether to adjust the parameters of the preparation process of the efficient nickel borate, it includes: The qualified rate of the prepared nickel boroacylate is compared with the preset qualified rate, wherein: If the qualified rate of the prepared nickel borate is lower than the preset qualified rate, it is determined that the preparation process parameters of the high-efficiency nickel borate need to be adjusted.

10. The process for preparing high-efficiency nickel boroacylate according to claim 9, characterized in that: The adjustment amount of the preset solubility degree is negatively correlated with the purity of nickel boroacylate, the adjustment amount of the preset increase rate is negatively correlated with the amount of nickel boroacylate produced, and the adjustment amount of the preset bubble number is negatively correlated with the amount of nickel boroacylate produced.

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