Calcium formate carbonyl synthesis process and method thereof

Abstract

The invention belongs to the technical field of calcium formate oxo-synthesis, and particularly relates to a calcium formate oxo-synthesis process and a calcium formate oxo-synthesis method, which are characterized in that through accurate raw material ratio, reaction condition control and operation step design, the molar ratio of a mixture, reaction temperature and time, filtration, concentration, crystallization and drying processes are optimized; the efficient synthesis of calcium formate carbonyl is realized. The optimized process not only improves the purity and the yield of the product, but also reduces the energy consumption and the production cost, and has remarkable economic and environmental advantages. Through detailed step description and operation parameter setting, important practical value and guiding significance are provided for technical progress in the field of calcium formate carbonyl synthesis.

Description

Technical Field

[0001] The invention belongs to the technical field of calcium formate carbonyl synthesis, and particularly relates to a calcium formate carbonyl synthesis process and a method thereof. Background Art

[0002] Calcium formate carbonyl is a compound containing a carbonyl group (C=O) coordinated with a formic acid group (HCOO-), with the chemical formula Ca(HCOO)2. It usually exists as a white crystalline solid. Calcium formate carbonyl has important applications as a catalyst in chemical synthesis, especially in carbonylation reactions. Carbonylation reactions are an important class of organic synthesis reactions, which are usually used to synthesize compounds such as esters, alcohols, and ethers. Calcium formate carbonyl as a catalyst can promote the progress of these reactions and improve the selectivity and yield of the reactions. In addition, it also acts as an alkaline or oxidative catalyst in other organic synthesis reactions and is widely used in the chemical industry and laboratory research.

[0003] The traditional calcium formate carbonyl synthesis process has many technical challenges and efficiency problems, such as insufficient precision in the raw material ratio leading to low reaction efficiency, inaccurate control of reaction conditions leading to unstable product quality, poor results in the filtration, concentration, crystallization, separation and drying processes, an imperfect quality control system, difficulty in ensuring product purity and high production costs. At the same time, there is a need for improvement in environmental friendliness and process flexibility. Summary of the invention

[0004] In order to make up for the deficiencies of the prior art, the embodiments of the present application provide a calcium formate carbonyl synthesis process and method thereof, thereby solving a series of problems in the prior art, such as low raw material utilization, unstable product quality, low purity, high energy consumption, high cost and insufficient environmental friendliness.

[0005] In order to solve the above technical problems, the present invention provides the following technical solution: a calcium formate carbonyl synthesis process, characterized in that: the calcium formate carbonyl synthesis process comprises the following steps:

[0006] 1) Raw material preparation: formic acid, calcium hydroxide, and deionized water are mixed in a molar ratio of 1:8-2:2:1:5-10;

[0007] 2) Reaction: stirring the mixture at 60-80° C. for 2-4 hours to obtain a calcium formate solution;

[0008] 3) Filtration: Filter the reaction solution through a 100-200 mesh filter cloth to remove insoluble matter;

[0009] 4) Concentration: The filtrate is evaporated and concentrated under reduced pressure to a solid content of 50-60%;

[0010] 5) Crystallization: Cool the concentrated solution to 0-5°C and allow to crystallize for 4-8 hours;

[0011] 6) Separation: centrifugation to separate calcium formate crystals;

[0012] 7) Drying: Dry the crystals at 50-60° C. for 4-6 hours to obtain a calcium formate product.

[0013] Preferably: in step 1), the molar ratio of formic acid, calcium hydroxide and deionized water is preferably 2:1:8.

[0014] Preferably: in the step 2), the reaction temperature is preferably 70° C., and the reaction time is preferably 3 hours.

[0015] Preferably, in step 3), 150 mesh filter cloth is used for filtration.

[0016] Preferably: in the step 4), the concentration is carried out under a vacuum degree of 0.05-0.08 MPa.

[0017] Preferably: in the step 5), the crystallization temperature is preferably 2° C., and the crystallization time is preferably 6 hours.

[0018] Preferably, in step 6), the rotation speed of the centrifugal separation is 1000-1500 r / min, and the time is 10-15 minutes.

[0019] Preferably: in step 7), the drying temperature is preferably 55° C., and the drying time is preferably 5 hours.

[0020] Preferably: the calcium formate carbonyl synthesis method comprises the following steps:

[0021] 1) Mix formic acid and calcium hydroxide in a molar ratio of 2:1, and add 8 times the molar amount of deionized water;

[0022] 2) stirring and reacting at 70° C. for 3 hours to obtain a calcium formate solution;

[0023] 3) Filter the reaction solution through a 150-mesh filter cloth;

[0024] 4) Evaporation and concentration under a vacuum degree of 0.06 MPa to a solid content of 55%;

[0025] 5) Cool the concentrated solution to 2°C and allow to crystallize for 6 hours;

[0026] 6) centrifugation at 1200 r / min for 12 minutes to obtain calcium formate crystals;

[0027] 7) Drying at 55° C. for 5 hours to obtain a calcium formate product with a purity of ≥99%.

[0028] Preferably: in the step 2), the stirring speed is 300-500 r / min.

[0029] In the step 4), the concentration temperature is 50-60°C.

[0030] In the step 5), the stirring speed during the crystallization process is 50-100 r / min.

[0031] In the step 7), drying is performed in a hot air circulation oven.

[0032] One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:

[0033] 1. The present invention solves the problem of low reaction efficiency caused by improper raw material ratio in the existing process by setting a precise raw material molar ratio (formic acid: calcium hydroxide: deionized water = 2:1:8).

[0034] 2. The present invention solves the problem of unstable product quality caused by lax control of reaction conditions in the existing process by setting specific reaction temperature (70°C), time (3 hours) and stirring speed (300-500r / min).

[0035] 3. The present invention solves the problem of low product purity caused by poor filtering effect in the existing process by using a 150-mesh filter cloth for filtration.

[0036] 4. The present invention solves the problems of high energy consumption and easy loss of product quality in the existing process of concentration by setting a specific vacuum degree (0.06MPa) and temperature (50-60°C) for concentration.

[0037] 5. The present invention solves the problems of unstable crystallization quality and low yield in the existing process by setting precise crystallization temperature (2°C), time (6 hours) and stirring speed (50-100r / min). DETAILED DESCRIPTION

[0038] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0039] It should be noted that the terms “vertical”, “horizontal”, “up”, “down”, “left”, “right” and similar expressions used in this document are only for illustrative purposes and do not represent the only implementation method.

[0040] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by technicians in the technical field to which the present invention belongs; the terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention; the term "and / or" used herein includes any and all combinations of one or more related listed items.

[0041] A calcium formate carbonyl synthesis process, characterized in that: the calcium formate carbonyl synthesis process comprises the following steps:

[0042] 1) Raw material preparation: Mix formic acid, calcium hydroxide and deionized water in a molar ratio of 1.8-2.2:1:5-10;

[0043] 2) Reaction: stirring the mixture at 60-80° C. for 2-4 hours to obtain a calcium formate solution;

[0044] 3) Filtration: Filter the reaction solution through a 100-200 mesh filter cloth to remove insoluble matter;

[0045] 4) Concentration: The filtrate is evaporated and concentrated under reduced pressure to a solid content of 50-60%;

[0046] 5) Crystallization: Cool the concentrated solution to 0-5°C and allow to crystallize for 4-8 hours;

[0047] 6) Separation: centrifugation to separate calcium formate crystals;

[0048] 7) Drying: Dry the crystals at 50-60° C. for 4-6 hours to obtain a calcium formate product.

[0049] In the step 1), the molar ratio of formic acid, calcium hydroxide and deionized water is preferably 2:1:8.

[0050] In the step 2), the reaction temperature is preferably 70° C. and the reaction time is preferably 3 hours.

[0051] In the step 3), 150 mesh filter cloth is used for filtration.

[0052] In the step 4), the concentration is carried out under a vacuum degree of 0.05-0.08 MPa.

[0053] In the step 5), the crystallization temperature is preferably 2° C., and the crystallization time is preferably 6 hours.

[0054] In the step 6), the rotation speed of the centrifugal separation is 1000-1500 r / min, and the time is 10-15 minutes.

[0055] In the step 7), the drying temperature is preferably 55° C. and the drying time is preferably 5 hours.

[0056] In this embodiment, this calcium formate carbonyl synthesis process has many advantages. First, by optimizing the raw material ratio and using a molar ratio of formic acid, calcium hydroxide and deionized water of 2:1:8, the reaction can be ensured to be fully carried out and the waste of raw materials can be avoided. Secondly, under the condition of 70°C reaction for 3 hours, not only can the reaction be ensured to be complete, but also energy can be effectively saved. The use of 150 mesh filter cloth can significantly improve the filtration effect and remove insoluble matter, thereby improving the purity of the product. Concentrating under a vacuum degree of 0.05-0.08MPa can speed up the concentration speed and reduce the decomposition of heat-sensitive substances. During the crystallization process, by crystallizing at 2°C for 6 hours, larger and uniform crystals can be obtained, which improves the product quality. In the separation stage, centrifugation at 1000-1500r / min for 10-15 minutes can effectively separate crystals and mother liquor. Finally, under the reasonable parameters of drying at 55°C for 5 hours, the product can be fully dried without causing product decomposition. Overall, these optimized process parameters can significantly improve the quality, production efficiency and yield of calcium formate products, while reducing energy consumption and costs, bringing many benefits to the production process.

[0057] A method for synthesizing calcium formate carbonyl, characterized in that the method comprises the following steps:

[0058] 1) Mix formic acid and calcium hydroxide in a molar ratio of 2:1, and add 8 times the molar amount of deionized water;

[0059] 2) stirring and reacting at 70° C. for 3 hours to obtain a calcium formate solution;

[0060] 3) Filter the reaction solution through a 150-mesh filter cloth;

[0061] 4) Evaporation and concentration under a vacuum degree of 0.06 MPa to a solid content of 55%;

[0062] 5) Cool the concentrated solution to 2°C and allow to crystallize for 6 hours;

[0063] 6) centrifugation at 1200 r / min for 12 minutes to obtain calcium formate crystals;

[0064] 7) Drying at 55° C. for 5 hours to obtain a calcium formate product with a purity of ≥99%.

[0065] In the step 2), the stirring speed is 300-500 r / min.

[0066] In the step 4), the concentration temperature is 50-60°C.

[0067] In the step 5), the stirring speed during the crystallization process is 50-100 r / min.

[0068] In the step 7), drying is performed in a hot air circulation oven.

[0069] In this embodiment, the key steps in the calcium formate carbonyl synthesis process include: mixing formic acid and calcium hydroxide in a 2: 1 molar ratio and adding an appropriate amount of deionized water, which helps to carry out efficient reaction at 70°C. Impurities can be effectively removed by filtering the reaction solution through a 150-mesh filter cloth. Evaporation and concentration to 55% solid content under low vacuum helps to increase the concentration of the product. Standing crystallization for 6 hours at low temperature, combined with centrifugal separation operation, helps to obtain calcium formate crystals with a purity of up to 99%. Finally, drying in a hot air circulation oven at 55°C for 5 hours ensures the stability and high purity of the product. Throughout the process, precise operating conditions and step control, such as stirring speed and temperature control, can effectively improve the yield and product quality of calcium formate carbonyl synthesis.

[0070] Although the present invention has been disclosed as above in the form of a preferred embodiment, it is not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the definition of the claims.

Claims

1. A calcium formate carbonyl synthesis process, characterized in that: The calcium formate carbonyl synthesis process comprises the following steps: 1) Raw material preparation: Mix formic acid, calcium hydroxide and deionized water in a molar ratio of 1.8-2.2:1:5-10; 2) Reaction: stirring the mixture at 60-80° C. for 2-4 hours to obtain a calcium formate solution; 3) Filtration: Filter the reaction solution through a 100-200 mesh filter cloth to remove insoluble matter; 4) Concentration: The filtrate is evaporated and concentrated under reduced pressure to a solid content of 50-60%; 5) Crystallization: Cool the concentrated solution to 0-5°C and allow to crystallize for 4-8 hours; 6) Separation: centrifugation to separate calcium formate crystals; 7) Drying: Dry the crystals at 50-60° C. for 4-6 hours to obtain a calcium formate product.

2. A calcium formate carbonyl synthesis process according to claim 1, characterized in that: In the step 1), the molar ratio of formic acid, calcium hydroxide and deionized water is preferably 2:1:

8.

3. A calcium formate carbonyl synthesis process according to claim 1, characterized in that: In the step 2), the reaction temperature is preferably 70° C. and the reaction time is preferably 3 hours.

4. A calcium formate carbonyl synthesis process according to claim 1, characterized in that: In the step 3), 150 mesh filter cloth is used for filtration.

5. A calcium formate carbonyl synthesis process according to claim 1, characterized in that: In the step 4), the concentration is carried out under a vacuum degree of 0.05-0.08 MPa.

6. A calcium formate carbonyl synthesis process according to claim 1, characterized in that: In the step 5), the crystallization temperature is preferably 2° C., and the crystallization time is preferably 6 hours.

7. A calcium formate carbonyl synthesis process according to claim 1, characterized in that: In the step 6), the rotation speed of the centrifugal separation is 1000-1500 r / min, and the time is 10-15 minutes.

8. A calcium formate carbonyl synthesis process according to claim 1, characterized in that: In the step 7), the drying temperature is preferably 55° C. and the drying time is preferably 5 hours.

9. A method for carbonyl synthesis of calcium formate, characterized in that: The calcium formate carbonyl synthesis method comprises the following steps: 1) Mix formic acid and calcium hydroxide in a molar ratio of 2:1, and add 8 times the molar amount of deionized water; 2) stirring and reacting at 70° C. for 3 hours to obtain a calcium formate solution; 3) Filter the reaction solution through a 150-mesh filter cloth; 4) Evaporation and concentration under a vacuum degree of 0.06 MPa to a solid content of 55%; 5) Cool the concentrated solution to 2°C and allow to crystallize for 6 hours; 6) centrifugation at 1200 r / min for 12 minutes to obtain calcium formate crystals; 7) Drying at 55° C. for 5 hours to obtain a calcium formate product with a purity of ≥99%.

10. A method for carbonyl synthesis of calcium formate according to claim 9, characterized in that: In the step 2), the stirring speed is 300-500 r / min. In the step 4), the concentration temperature is 50-60°C; In the step 5), the stirring speed during the crystallization process is 50-100 r / min; In the step 7), drying is performed in a hot air circulation oven.