Synthetic vitamin E recrystallization, filtration, washing and drying three-in-one

2023/03/19

Vitamin E succinate is a natural vitamin E derivative. It is formed by esterification of succinic acid and the 6-hydroxyl group of α-tocopherol. It not only retains the biological activity of α-tocopherol. Studies have shown that vitamin E succinate Ester has good anti-tumor activity, and can prevent and treat various tumors such as gastric cancer, leukemia, prostate cancer, pancreatic cancer, breast cancer, and colorectal cancer. As a solid form of vitamin E, it is widely used in medicine, health care products, food and cosmetics. In developed countries such as Europe and the United States, the application of vitamin E succinate in health food is very common, and the vitamin E used in almost all nutritional supplements in the form of tablets and hard capsules is vitamin E succinate.



The filter washing and drying machine is referred to as "three-in-one". It is an equipment that completes filtration, washing, drying and other processes in a closed container. It was developed and applied abroad in the 1960s. Due to the high price of imported equipment, domestic pharmaceutical, food, and chemical industries have seldom used it.

According to market demand and customer requirements, our company has carried out a lot of design and development work, and finally successfully developed a conical filter, washing and drying three-in-one multifunctional equipment, and successfully applied for patents (patent numbers: 202022908020.2, 202022906527.4), breaking foreign monopoly, A great improvement in the technical performance of the equipment has been achieved, and the price of the three-in-one equipment has been greatly reduced.
Due to the use of organic solvents in the production of vitamin E succinate, there are certain safety and occupational health risks. The traditional process equipment is intermittent production, and the labor intensity of employees is relatively high. There is an urgent need to improve production conditions and reduce safety risks. Wuxi ZhangHua produced the new filter, washing and drying three-in-one using vitamin E succinate, which successfully replaced the conventional process of centrifuge and boiling dryer, achieved good economic and environmental benefits, and the production is more in line with GMP requirements.





Analysis of the old production process of vitamin E derivatives
D-α-tocopherol and succinic acid are esterified, recrystallized, filtered, pulverized, and dried to prepare vitamin E succinate. The original process uses a centrifuge to filter and wash, and the filter cake is pulverized by a oscillating granulator. Then dry it with a boiling dryer. This process has the following disadvantages:
(1) High security risk
Using a centrifuge to filter, because the materials processed by the centrifuge are flammable and explosive, it is easy to cause combustion and explosion accidents. And because of its high speed, if the operation is careless or violates the regulations, it will contact with the material in the rotating centrifuge drum, which will cause accidents of severed fingers and arms.

In addition, drum rupture, drum displacement, and manhole cover flying out due to various reasons will also cause serious casualties.
(2) Large environmental pollution
Since the wet product contains 40% solvent by mass, it will volatilize into the atmosphere after being boiled and dried, and cannot be recovered effectively, causing great environmental pollution.
(3) It cannot be airtight for production and does not comply with GMP
Material transfer operation is required between the steps of filtration, crushing, and drying. The automation level is low, and more personnel are required for each shift operation. During the material transfer operation, there are risks of occupational diseases such as solvents and dust, foreign matter control and other quality control difficulties, and GMP management is difficult. .


(4) Large footprint
The old process layout requires a centrifuge, a swing granulator, and a boiling dryer, and the production equipment occupies a large area.





New technological process of vitamin E derivatives - new three-in-one filtration, washing and drying
After esterification of d-α-tocopherol and succinic acid, recrystallization, enter the three-in-one, complete filtration, washing, drying in the same equipment, and dry to obtain the finished product.
(1) Filtration process
Add the crystallization solution into the three-in-one, and pressurize the three-in-one to filter with nitrogen. In order to speed up the filtration, you can also vacuumize the filtrate tank.

If air leakage (and cracks) are found in the filter cake, the stirring paddle can be lowered and reversed to flatten the surface of the filter cake.
(2) Washing process
After the filtration, add a solvent to wash, and the residual mother liquor on the crystallization surface of the filter cake can be washed clean to remove impurities and improve product quality.
(3) Drying process
After the filtration, turn on the three-in-one stirring, turn on the vacuum system, and dry the solvent contained in the filter cake. In order to speed up the drying, you can heat it with hot water in the three-in-one jacket.

Equipped with a solvent recovery system during drying, the vapor discharged from the solvent after drying enters the condensation recovery device, and the solvent can be used mechanically after condensation, reducing solvent loss. After the drying is finished, the product can be obtained after sampling and testing are qualified.



Filtration, washing and drying three-in-one application in the production of vitamin E derivatives Technical advantages
The multifunctional filter washing and drying machine can carry out the continuous closed operation of the whole process of filtering, washing and drying in the same container, and the material can be discharged automatically. Compared with the traditional process, it has the following advantages:
(1) The production process is fully enclosed
The fully enclosed production process from the beginning of crystallization to the end of drying, this set of equipment is a fully enclosed operating system, the production process is more in line with GMP requirements, eliminating dust volatilization factors, controlling foreign matter pollution, and reducing the risk of microbial contamination.


(2) Safe and secure
The use of a filter washer-dryer instead of a centrifuge to filter the filter eliminates the safety risk of the centrifuge. The filter washing and drying machine can be filled with nitrogen protection during the filtration process, and the safety risk is low. Due to the fully enclosed operation of this production system, it can completely avoid the pollution of the solvent in the production process to the air of the operating environment, and at the same time reduce the occurrence of poisoning accidents caused by contact with toxic substances.

This advantage is even more important today when the voice of safety and occupational health is getting higher and higher.
(3) more environmentally friendly
Because the entire production system is a fully closed system operation, materials and solvents can be recovered almost 100% completely, avoiding waste caused by material omission, residue and solvent volatilization, which has great economic benefits, especially in the treatment of materials and use This is especially true at higher solvent values.
(4) Simple operation and high degree of automation
Each process is carried out in stages, and the safety measures are complete. The operators can complete the operation after simple training, and the labor intensity is greatly reduced.


(5) Product quality improvement
Because this equipment can re-stir and suspend the filter cake during the washing operation, the impurities in the filter cake can be cleaned thoroughly, which is conducive to improving product quality.
(6) All operations can be performed using the same system
Filtration, washing, and drying can be completed in the same system, and the workshop space has also been utilized to the maximum. In the era when every inch of land is expensive, reducing the floor space can save a lot of capital investment.
(7) Cleaner production
The filter washing and drying machine can operate in a closed manner, and is equipped with a dust collector to completely collect the dust generated after drying, which can meet the production operation requirements of high cleanliness.


(8) Realize online cleaning
The filter washing and drying machine is equipped with a spray ball, which can easily realize online cleaning operation. Compared with traditional equipment, it can reduce solvent volatilization and safety risks during cleaning.


In the vitamin E succinate production line with an annual output of 200 tons, the use of Wuxi ZhangHua's three-in-one equipment has reduced a large amount of solvent loss, reduced safety risks, improved automation, and reduced operators, with an annual economic benefit of 2 million above. Due to the airtight operation of the equipment, the product quality is improved, and the occupied area is small, indicating that the use of the filter washing and drying machine has achieved good economic and environmental benefits, and the production is more in line with GMP requirements.


Organic solvents are used in the production of vitamin E derivatives. The traditional process equipment is intermittent production, and the labor intensity of employees is relatively high. There is an urgent need to improve production conditions and reduce safety risks. Wuxi ZhangHua produced the new filter, washing and drying three-in-one using vitamin E succinate, which successfully replaced the conventional process of centrifuge and boiling dryer, achieved good economic and environmental benefits, and the production is more in line with GMP requirements.

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