Preparation method for stannous neodecanoate, and reactor

Abstract

The present invention relates to the technical field of chemical production, and relates in particular to a preparation method for stannous neodecanoate, and a reactor. The method comprises: adding, according to a preset ratio, metallic tin and hydrochloric acid into a reactor for reaction, and obtaining a solution; preparing a sodium carbonate solution, adding said solution into the sodium carbonate solution for reaction, performing solid-liquid separation by a centrifuge, and obtaining tin powder; adding the tin powder and neodecanoic acid into a reactor according to a ratio, stirring, heating with steam, turning off the steam after the temperature rises to 105°C, cooling to room temperature, and obtaining a crude stannous neodecanoate; pressurizing the reactor by using nitrogen, pressing the crude stannous neodecanoate from the reactor into a filter buffer tank, performing filtering, and obtaining stannous neodecanoate. The present process has a relatively mild reaction, avoiding unpredictable reaction risks during the production process. In addition, the stannous neodecanoate produced by the present process has stable quality and color and a yield of more than 98%, which can reduce production and operation costs.

Description

Preparation method and reactor of stannous neodecanoate Technical Field

[0001] The present invention relates to the technical field of chemical production, in particular to a preparation method and a reactor of stannous neodecanoate. Background Art

[0002] With the diversification and diversification of polyurethane application scenarios, the production capacity of polyurethane products is increasing year by year, and the annual consumption of stannous octoate as a metal catalyst is also increasing year by year. Stannous octoate, also known as tin octoate, is a chemical substance with a molecular formula of C4H9Sn(OH)2 and a chemical name of dibutylstannous octoate. It is an organic tin compound with a common structure of one tin atom combined with two octanoic acid groups. Stannous octoate is a colorless to slightly yellow liquid with certain toxicity. However, from November 23, 2023, the list of banned substances will be expanded, and polyurethane foam containing stannous octoate will not be able to pass certification.

[0003] The existing production process is highly dangerous. For example, the acidic substances in the existing stannous decanoate process and the violent exothermic reaction of stannous decanoate during the production process when sodium hydroxide is added to generate stannous oxide pose safety risks and occupational health hazards to production operators.

[0004] The stannous neodecanoate of the present invention can replace stannous octoate and be applied in the polyurethane product industry, thus making up for the current deficiency of stannous octoate.

[0005] Summary of the Invention

[0006] The purpose of the present invention is to provide a preparation method and reactor of stannous neodecanoate, aiming to make the reaction mild and avoid the risk of unpredictable reaction during the production process; the stannous neodecanoate produced by this process has stable quality and color, a yield of more than 98%, and can reduce production and operation costs.

[0007] To achieve the above object, the present invention provides a method for preparing stannous neodecanoate, comprising adding metallic tin and hydrochloric acid according to a preset ratio into a reactor to react and obtain a solution;

[0008] Prepare a sodium carbonate solution, add the solution into the sodium carbonate solution to react, and separate the solid and liquid by a centrifuge to obtain tin powder;

[0009] Tin powder and neodecanoic acid were added into a reactor according to a ratio and stirred, and steam was applied to heat the reactor until the temperature reached 105°C, and then the steam was turned off and the reactor was cooled to room temperature to obtain crude stannous neodecanoate.

[0010] The reactor is pressurized with nitrogen, and the crude stannous neodecanoate in the reactor is pressed into a filter buffer tank, and filtered to obtain stannous neodecanoate.

[0011] The specific steps of reacting metallic tin and hydrochloric acid according to a preset ratio to obtain a solution include:

[0012] The metallic tin is transported to the reactor through a pipe chain automatic feeder, and the hydrochloric acid is transported to the reactor after being measured by a flow meter through a feed pump;

[0013] Heat with steam to make the metal tin and hydrochloric acid react. When the temperature rises to 90-95°C, keep it warm. During the heating period, turn on the vacuum pump. After keeping warm for 5 hours, turn off the vacuum pump.

[0014] Nitrogen was slowly introduced into the reactor to relieve the pressure. When the temperature in the reactor was cooled to 50-60° C. by passing condensed water through the coil, the content of the reactants was detected to make the Baume degree reach above 55, thereby obtaining a solution.

[0015] The preset ratio of the metallic tin and the hydrochloric acid is 25% to 35% metallic tin and 65% to 75% hydrochloric acid.

[0016] The specific method of heating by steam is as follows: the steam opening degree is 30%, and then increased by 25% every 15 minutes, and the maximum steam opening degree is 80%.

[0017] Wherein, the vacuum pressure of the vacuum pump during the heating period is -0.09 to -0.095 MPa.

[0018] The steps of preparing a sodium carbonate solution, adding the solution into the sodium carbonate solution for reaction, and performing solid-liquid separation by a centrifuge to obtain tin powder include:

[0019] Add water or pure water into the reactor, then add sodium carbonate into the reactor, start the reactor and stir to prepare the sodium carbonate solution;

[0020] The above solution was added to a sodium carbonate solution and reacted for 2 h. The ratio of the solution to the sodium carbonate solution was 1:6 to obtain a mixed solution.

[0021] The mixed liquid is separated into solid and liquid by a centrifuge to obtain tin powder.

[0022] In which, the reactor includes a support assembly, multiple feeding assemblies, a reaction assembly and a temperature control assembly, the support assembly includes a base and a support frame, the support frame is fixedly connected to the base and is located on the top of the base, the reaction assembly includes a reaction tank, a stirring motor and a stirring rod, the reaction tank has a heating layer and a reaction chamber, the heating layer is arranged outside the reaction chamber, the stirring motor is fixedly connected to the reaction tank and is located on one side of the reaction tank, the stirring rod is fixedly connected to the output end of the stirring motor and is located in the reaction tank, multiple feeding assemblies are arranged on the top of the reaction tank, the temperature control assembly includes a steam generator, a spiral tube, a vacuum pump, a detector, a cooling tank and a cooler, the steam generator is arranged on one side of the heating layer, the spiral tube is arranged at the bottom of the reaction tank, the vacuum pump is arranged on one side of the reaction tank, the detector is fixed on the reaction tank, the cooler is arranged on one side of the spiral tube, and the cooling tank is arranged at the bottom of the spiral tube.

[0023] Wherein, the steam generator includes an evaporator, a connecting pipe, multiple nozzles and a reflux pipe. The evaporator is arranged on one side of the reaction tank. The connecting pipe is connected to the evaporator. The multiple nozzles are connected to the connecting pipe and are located around the heating layer. The reflux pipe is connected to the bottom of the heating layer and is connected to the evaporator.

[0024] The present invention provides a method and reactor for preparing stannous neodecanoate, comprising: adding metallic tin and hydrochloric acid to a reactor according to a preset ratio for reaction to obtain a solution; preparing a sodium carbonate solution, adding the solution to the sodium carbonate solution for reaction, and performing solid-liquid separation in a centrifuge to obtain tin powder; adding the tin powder and neodecanoic acid to a reactor according to a ratio, stirring, heating with steam, heating the reactor until the temperature rises to 105° C., then turning off the steam and cooling the reactor to room temperature to obtain a crude stannous neodecanoate product; pressurizing the reactor with nitrogen, and pressurizing the crude stannous neodecanoate product in the reactor into a filter buffer tank, filtering, and obtaining the stannous neodecanoate product. This process has a relatively mild reaction, avoiding the risk of unpredictable reactions during the production process; the stannous neodecanoate produced by this process has stable quality and color, a yield of over 98%, and can reduce production and operating costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0026] FIG1 is a flow chart of a method for preparing stannous neodecanoate according to a first embodiment of the present invention.

[0027] FIG2 is a flow chart of the first embodiment of the present invention, in which metallic tin and hydrochloric acid are added into a reactor according to a preset ratio to react and obtain a solution.

[0028] FIG3 is a flow chart of the first embodiment of the present invention, wherein a sodium carbonate solution is prepared, the solution is added to the sodium carbonate solution for reaction, and solid-liquid separation is performed by a centrifuge to obtain tin powder.

[0029] FIG4 is a structural diagram of a reactor according to a second embodiment of the present invention.

[0030] FIG5 is a right side structural diagram of a reactor according to a second embodiment of the present invention.

[0031] FIG6 is a cross-sectional structural diagram of a reactor according to a second embodiment of the present invention.

[0032] FIG. 7 is a partial enlarged view of detail A in FIG. 6 .

[0033] Support assembly 101, loading assembly 102, reaction assembly 103, temperature control assembly 104, base 105, support frame 106, reaction tank 107, stirring motor 108, stirring rod 109, heating layer 110, reaction chamber 111, steam generator 112, spiral tube 113, vacuum pump 114, detector 115, cooling tank 116, cooler 117, evaporator 118, connecting pipe 119, multiple nozzles 120, reflux pipe 121, temperature sensor 122, pressure sensor 123, sealing tube 124, circulation pump 125, cooling box 126, preheating box 127, box body 128, heat sink 129, preheating discharge box 130, second spiral tube 131, heat conducting plate 132, and agitator 133. DETAILED DESCRIPTION

[0034] The following describes embodiments of the present invention in detail, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present invention, and are not to be construed as limiting the present invention.

[0035] First embodiment

[0036] Referring to Figures 1 to 3, the present invention provides a method for preparing stannous neodecanoate, comprising:

[0037] S101: adding metallic tin and hydrochloric acid according to a preset ratio into a reactor to react and obtain a solution;

[0038] Specific steps include;

[0039] S201: The metallic tin is transported to the reactor through the automatic tube chain feeder, and the hydrochloric acid is transported to the reactor after being measured by the flow meter through the feed pump;

[0040] The preset ratio of the metallic tin and the hydrochloric acid is 25% to 35% of the metallic tin and 65% to 75% of the hydrochloric acid.

[0041] S202 is heated by steam to react the metal tin and hydrochloric acid. When the temperature rises to 90-95°C, the temperature is kept warm. During the heating period, the vacuum pump 114 is turned on. After the temperature is kept warm for 5 hours, the vacuum is turned off.

[0042] The specific method of heating by steam is as follows: the steam opening degree is 30%, and then increased by 25% every 15 minutes, and the maximum steam opening degree is 80%.

[0043] During the heating period, the vacuum pump 114 is turned on to maintain a vacuum pressure of -0.09 to -0.095 MPa.

[0044] Slowly introduce nitrogen into the S203 reactor to release the pressure. When the coil in the reactor is cooled to 50-60°C by passing condensed water, the content of the reactants is detected to make the Baume degree reach above 55 to obtain a solution.

[0045] S102: preparing a sodium carbonate solution, adding the solution to the sodium carbonate solution for reaction, and performing solid-liquid separation by a centrifuge to obtain tin powder;

[0046] In addition to sodium carbonate, the present invention can also use sodium bicarbonate as a raw material. Here, sodium bicarbonate is used as the raw material for preparation, and the specific steps include:

[0047] S301: Add water or pure water into the reactor, then add sodium bicarbonate into the reactor, start the reactor and stir to prepare the sodium bicarbonate solution;

[0048] S302: adding the above solution into sodium bicarbonate solution and reacting for 2 hours, with the ratio of the solution to the sodium carbonate solution being 1:6, to obtain a mixed solution;

[0049] S303: The mixed liquid is separated into solid and liquid by a centrifuge to obtain tin powder.

[0050] In addition, the present invention can also use sodium hydroxide as a raw material for production. The specific method will not be repeated here. The difference between using sodium carbonate and sodium bicarbonate and sodium hydroxide is that the reaction of sodium carbonate and sodium bicarbonate with stannous chloride solution is an endothermic reaction, which is relatively mild, while the reaction of sodium hydroxide with stannous chloride solution is an exothermic reaction, which is relatively violent, but tin powder can be finally obtained without affecting product quality.

[0051] S103: adding tin powder and neodecanoic acid in a proportioned manner into a reactor, stirring, and heating with steam until the temperature rises to 105° C., then turning off the steam and cooling to room temperature to obtain crude stannous neodecanoate;

[0052] S104 pressurizes the reactor with nitrogen, and pressurizes the crude stannous neodecanoate in the reactor into the filter buffer tank, and obtains stannous neodecanoate after filtration.

[0053] The above reaction equation is as follows;

[0054] The stannous neodecanoate produced in this project has a milder reaction than the violent exothermic reaction in the stannous chloride production process, thus avoiding unpredictable reaction risks during the production process, such as environmental hazards caused by material spillage due to violent reactions and waste gas pollution caused by violent reactions.

[0055] The stannous neodecanoate produced in this project has unfavorable factors such as unstable quality and color and low yield produced by stannous oxide as raw material. The stannous neodecanoate produced by this process has stable quality and color, and a yield of more than 98%, which can reduce production and operation costs.

[0056] Second embodiment

[0057] Please refer to Figures 4 to 7. Figure 4 is a structural diagram of the reactor of the second embodiment of the present invention. Figure 5 is a right structural diagram of the reactor of the second embodiment of the present invention. Figure 6 is a cross-sectional structural diagram of the reactor of the second embodiment of the present invention. Figure 7 is a partial enlarged view of detail A of Figure 6. On the basis of the first embodiment, the present invention also provides a reactor, which includes a support component 101, multiple feeding components 102, a reaction component 103 and a temperature control component 104. The support component 101 includes a base 105 and a support frame 106. The support frame 106 is fixedly connected to the base 105 and is located on the top of the base 105. The reaction component 103 includes a reaction tank 107, a stirring motor 108 and a stirring rod 109. The reaction tank 107 has a heating layer 110 and a reaction chamber 111. The heating layer 110 is arranged on the outside of the reaction chamber 111. The stirring motor 108 is fixedly connected to the reaction tank 107 and is located on one side of the reaction tank 107. The stirring rod 109 is fixedly connected to the reaction tank 107 and is located on the side of the reaction tank 107. The output end of the stirring motor 108 is fixedly connected and located in the reaction tank 107. Multiple feeding components 102 are arranged on the top of the reaction tank 107. The temperature control component 104 includes a steam generator 112, a spiral tube 113, a vacuum pump 114, a detector 115, a cooling tank 116 and a cooler 117. The steam generator 112 is arranged on one side of the heating layer 110, the spiral tube 113 is arranged at the bottom of the reaction tank 107, the vacuum pump 114 is arranged on one side of the reaction tank 107, the detector 115 is fixed on the reaction tank 107, the cooler 117 is arranged on one side of the spiral tube 113, and the cooling tank 116 is arranged at the bottom of the spiral tube 113.

[0058] In this embodiment, the base 105 can provide support for the support frame 106, so that the reaction tank 107 serves as a reaction site, and the reaction chamber 111 on the reaction tank 107 is used for chemical reaction, and steam can be introduced into the reaction chamber 111 through the steam generator 112 for heating. In specific use, various raw materials are added to the reaction tank 107 through the loading assembly 102, and then the stirring motor 108 is started to drive the stirring rod 109 for mixing. The steam generator 112 can heat the reaction tank 107 so that the raw materials are heated within a preset temperature range. The temperature and pressure of the reaction tank 107 can be detected by the detector 115. After the reaction is completed, the valve at the bottom of the reaction tank 107 can be opened so that the raw materials can be passed into the spiral tube 113 for cooling, and finally placed through the cooling tube. The cooler 117 can perform heat exchange with the spiral tube 113, so that the raw materials can be processed conveniently and work efficiency can be improved.

[0059] The steam generator 112 includes an evaporator 118, a connecting pipe 119, a plurality of nozzles 120, and a return pipe 121. The evaporator 118 is disposed on one side of the reaction tank 107. The connecting pipe 119 is in communication with the evaporator 118. The plurality of nozzles 120 are in communication with the connecting pipe 119 and are located around the heating layer 110. The return pipe 121 is in communication with the bottom of the heating layer 110 and is connected to the evaporator 118. When the evaporator 118 is activated, steam can be generated, which can be distributed to the nozzles 120 through the connecting pipe 119, thereby heating the reaction tank 107 more evenly. The steam can then be returned to the evaporator 118 through the return pipe 121 for recycling.

[0060] The detector 115 includes a temperature sensor 122 and a pressure sensor 123, which are disposed in the reaction tank 107. The temperature sensor 122 and the pressure sensor 123 can detect parameters in the reaction tank 107, respectively, making it more convenient to use.

[0061] The cooler 117 includes a sealed tube 124, a circulation pump 125, a cooling box 126, and a preheating box 127. The sealed tube 124 is arranged outside the spiral tube 113, and the preheating box 127 is arranged on the top of the reaction tank 107. The circulation pump 125 is connected to the sealed tube 124 and the preheating box 127, and the cooling box 126 is connected to the preheating box 127 and the sealed tube 124. Cooling liquid is placed in the cooling box 126, and then the circulating pump 125 can pump the cooling liquid into the sealed tube 124 and contact the spiral tube 113 for heat exchange. Then, the heated liquid can enter the preheating box 127 to preheat the raw materials to be heated, thereby improving the utilization rate of heat.

[0062] The cooling box 126 includes a box body 128 and a heat sink 129. The heat sink 129 is fixedly connected to the box body 128 and is located outside the box body 128. The heat sink 129 can dissipate heat from the coolant in the box body 128.

[0063] The preheating box includes a preheating box 130, a second spiral tube 131, a heat conducting plate 132, and an agitator 133. The second spiral tube 131 is connected to the circulation pump 125 and the cooling box 126. The heat conducting plate 132 is arranged at the end of the second spiral tube 131. The preheating box 130 is arranged in the middle of the second spiral tube 131. The agitator 133 is arranged inside the box. The second spiral tube 131 can increase the contact area between the heated coolant and the heat conducting plate 132, thereby better conducting heat to the preheating box 130. The agitator 133 can stir the raw materials in the preheating box 130, so that the heat conduction effect is better.

[0064] The above disclosure is only a preferred embodiment of the present invention, and certainly cannot be used to limit the scope of the rights of the present invention. Ordinary technicians in this field can understand that all or part of the processes of the above embodiment and equivalent changes made in accordance with the claims of the present invention are still within the scope of the invention.

Claims

1. A method for preparing stannous neodecanoate, characterized in that: include: Adding metallic tin and hydrochloric acid according to a preset ratio into a reactor for reaction to obtain a solution; Prepare a sodium carbonate solution, put the solution into the sodium carbonate solution for reaction, and separate the solid and liquid by a centrifuge to obtain tin powder; Tin powder and neodecanoic acid are added into a reactor according to a ratio and stirred, and steam is applied for heating. After the temperature rises to 105° C., the steam is turned off and the temperature is lowered to room temperature to obtain a crude stannous neodecanoate; The reactor is pressurized with nitrogen, and the crude stannous neodecanoate in the reactor is pressed into the filter buffer tank, and stannous neodecanoate is obtained by filtration.

2. A method for preparing stannous neodecanoate as claimed in claim 1, characterized in that: The specific steps of reacting metallic tin and hydrochloric acid according to a preset ratio to obtain a solution include: The metallic tin is transported to the reactor through a pipe chain automatic feeder, and the hydrochloric acid is transported to the reactor through a feed pump after being measured by a flow meter; Steam is used for heating to make the metal tin and hydrochloric acid react. When the temperature rises to 90-95°C, the temperature is kept warm. During the heating period, a vacuum pump is turned on. After heating for 5 hours, the vacuum is turned off. Nitrogen was slowly introduced into the reactor to release the pressure. When the temperature in the reactor was cooled to 50-60°C by passing condensed water through the coil, the content of the reactants was detected to make the Baume degree reach above 55, thereby obtaining a solution.

3. A method for preparing stannous neodecanoate as claimed in claim 1, characterized in that: The preset ratio of the metallic tin and the hydrochloric acid is 25% to 35% of the metallic tin and 65% to 75% of the hydrochloric acid.

4. A method for preparing stannous neodecanoate as claimed in claim 2, characterized in that: The specific method of heating by steam is that the steam opening degree is 30%, and then increased by 25% every 15 minutes, and the maximum steam opening degree is 80%.

5. A method for preparing stannous neodecanoate as claimed in claim 4, characterized in that: During the heating period, the vacuum pressure of the vacuum pump is -0.09 to -0.095 MPa.

6. A method for preparing stannous neodecanoate as claimed in claim 5, characterized in that: The specific steps of preparing a sodium carbonate solution, putting the solution into the sodium carbonate solution for reaction, and separating the solid and liquid by a centrifuge to obtain tin powder include: Add water or pure water into the reactor, then add sodium carbonate into the reactor, start the reactor and stir to prepare the sodium carbonate solution; The above solution was added into sodium carbonate solution and reacted for 2 hours. The ratio of the solution to the sodium carbonate solution was 1:

6. A mixed solution is obtained; The mixed liquid is separated into solid and liquid by a centrifuge to obtain tin powder.

7. A reactor, applied to the method for preparing stannous neodecanoate according to claim 6, characterized in that: The reactor comprises a supporting assembly, a plurality of feeding assemblies, a reaction assembly and a temperature control assembly, wherein the supporting assembly comprises a base and a supporting frame, wherein the supporting frame is fixedly connected to the base and is located on the top of the base, wherein the reaction assembly comprises a reaction tank, a stirring motor and a stirring rod, wherein the reaction tank has a heating layer and a reaction chamber, wherein the heating layer is arranged outside the reaction chamber, wherein the stirring motor is fixedly connected to the reaction tank and is located on one side of the reaction tank, wherein the stirring rod is fixedly connected to the output end of the stirring motor and is located in the reaction tank, wherein a plurality of the feeding assemblies are arranged on the top of the reaction tank, wherein the temperature control assembly comprises a steam generator, a spiral tube, a vacuum pump, a detector, a cooling tank and a cooler, wherein the steam generator is arranged on one side of the heating layer, wherein the spiral tube is arranged on the bottom of the reaction tank, wherein the vacuum pump is arranged on one side of the reaction tank, wherein the detector is fixed on the reaction tank, wherein the cooler is arranged on one side of the spiral tube, and wherein the cooling tank is arranged on the bottom of the spiral tube.

8. A reactor as claimed in claim 7, characterized in that: The steam generator includes an evaporator, a connecting pipe, a plurality of nozzles and a reflux pipe. The evaporator is arranged on one side of the reaction tank. The connecting pipe is connected to the evaporator. The plurality of nozzles are connected to the connecting pipe and are located around the heating layer. The reflux pipe is connected to the bottom of the heating layer and is connected to the evaporator.

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