Synthetic vitamin E recrystallization filtration washing and drying machine

Synthetic vitamin E mainly refers to α -tocopherol and its ester derivatives (acetate esters, succinate esters), which have a wide range of uses. Besides being used as a vitamin, it also serves as an antioxidant to prevent oxidation in medicines, foods, cosmetics, feeds, and during the processing and storage of plastics.

Vitamin E succinate is a natural derivative of vitamin E. It is formed by the esterification of succinic acid with the 6-hydroxyl group of α -tocopherol. It not only retains the biological activity of α -tocopherol, but studies have shown that vitamin E succinate has good anti-tumor activity. It can prevent and treat various tumors such as gastric cancer, leukemia, prostate cancer, pancreatic cancer, breast cancer and colorectal cancer. As the solid form of vitamin E, it is more widely used in medicine, health products, food and cosmetics. In developed countries such as Europe and America, vitamin E succinate is widely used in health foods. Almost all vitamin E used in tablet and hard capsule forms of nutritional supplements is vitamin E succinate.

The filtration, washing and drying machine, abbreviated as "three-in-one", is a device that completes the processes of filtration, washing and drying in a closed container. It was developed and applied abroad in the 1960s. Due to the high price of imported equipment, it is less used in the domestic pharmaceutical, food and chemical industries. In response to market demands and customer requirements, our company has carried out extensive design and research and development work, and finally developed a multi-functional conical crystallization filtration, washing and drying integrated machine (patent number: (ZL 201721560677.6), breaking the foreign monopoly, achieving a significant improvement in the technical performance of the equipment, and greatly reducing the price of the three-in-one equipment.

Due to the use of organic solvents in the production of vitamin E succinate, there are certain safety and occupational health risks. 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 Shuangrui has successfully replaced the conventional process of centrifuge and fluidized bed dryer by applying a new type of three-in-one filtration, washing and drying technology to the production of vitamin E succinate, achieving good economic and environmental benefits and making the production more in line with GMP requirements.

Analysis of the Current Production Process of Vitamin E derivatives

Vitamin E succinate was prepared by esterification, recrystallization, centrifugation, crushing and drying of d-α -tocopherol and succinic acid. The original process involved centrifugation, washing, crushing of the filter cake by a swing granulator and then drying in a fluidized bed dryer. This process flow has the following disadvantages:

(1) High safety risk

When using a centrifuge for filtration, since the materials processed by the centrifuge are flammable and explosive, this can easily lead to the occurrence of combustion and explosion accidents. Moreover, due to its extremely high rotational speed, if operated carelessly or in violation of regulations, it may come into contact with the material inside the rotating centrifuge drum, causing accidents such as amputation of fingers or arms. In addition, drum breakage, drum displacement, and manhole cover flying out caused by various reasons can also lead to serious casualties.

(2) Severe environmental pollution

As the wet product contains 40% solvent by mass, after boiling and drying, it volatilizes into the atmosphere and cannot be effectively recovered, causing significant environmental pollution.

(3) It cannot be produced in a closed manner and does not comply with GMP

Between the steps of filtration, crushing and drying, there is a need for material transfer operations. The level of automation is low, and a large number of personnel are required for each shift. There are occupational disease risks such as solvents and dust during material transfer operations, and there are quality control difficulties such as foreign matter control. GMP management is difficult.

(4) It occupies a large area

The old process layout requires the support of centrifuges, swing granulators and fluidized bed dryers, and the production equipment occupies a relatively large area.

A new process flow for the refining, purification, filtration, washing and drying of vitamin raw material drug intermediates

After esterification and recrystallization of d-α -tocopherol and succinic acid, they enter the three-in-one process, where filtration, washing and drying are completed in the same equipment, and the finished product is obtained through drying.

(1) Filtration process

Add the crystalline liquid into the three-in-one unit. The three-in-one unit is then subjected to nitrogen pressure filtration. To accelerate the filtration process, vacuuming can also be carried out in the filtrate tank. If air leakage (and cracks) is 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 is completed, solvent washing is added to clean the residual mother liquor on the surface of the filter cake crystals, thereby removing impurities and improving product quality.

(3) Drying process

After the filtration is completed, start the three-in-one stirring and the vacuum system to dry the solvent contained in the filter cake. To speed up the drying process, hot water can be passed through the three-in-one jacket for heating. When drying, a solvent recovery system is equipped. The vapor discharged after the solvent is dried enters the condensation recovery device. After the solvent is condensed, it can be reused, reducing solvent loss. After the drying process is completed, if the sampling test is qualified, the product can be obtained.

Technical advantages of the intermediate refining, purification, filtration, washing and drying machine for vitamin raw materials

The multi-functional filtration, washing and drying machine can perform continuous and closed operations throughout the entire process of filtration, washing and drying in the same container, with automatic discharge. Compared with traditional processes, it has the following advantages:

(1) The production process flow is fully enclosed

From the start 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 and norms, eliminating dust volatilization factors, controlling foreign matter contamination, and reducing the risk of microbial contamination.

(2) Safety is guaranteed

The use of a filter washing dryer instead of a centrifuge for filtration eliminates the safety risks associated with the centrifuge. The filtration, washing and drying machine can be protected by nitrogen during the filtration process, with extremely low safety risks. As this production system operates in a fully enclosed manner, it can completely prevent the pollution of the operating environment air by solvents during the production process, and at the same time reduce the occurrence of poisoning accidents for operators caused by contact with toxic substances. Today, with the growing calls for safety and occupational health, this advantage becomes even more important.

(3) More environmentally friendly

Because the entire production system operates in a fully enclosed manner, materials and solvents can be nearly 100% completely recycled, avoiding waste caused by material omission, residue and solvent evaporation. This brings significant economic benefits, especially when handling materials and using solvents of high value.

(4) It is easy to operate and highly automated

Each process is carried out in stages, with complete safety measures. Operators can complete the operation after simple training, and the labor intensity is greatly reduced.

(5) Product quality has been improved

As this equipment can re-stir and suspend the filter cake during the washing operation, the impurities in the filter cake can be thoroughly cleaned, which is conducive to improving the product quality.

(6) All operations can be completed using the same system

Filtration, washing and drying can be completed in the same system, and the factory space is also utilized to the greatest extent. In an era where land is extremely precious, reducing the occupied area can save a large amount of capital investment.

(7) Clean production

The filtration, 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 filtration, washing and drying machine is equipped with spray balls, which can easily achieve online cleaning operations. Compared with traditional equipment, it can reduce solvent evaporation and safety risks during cleaning.

After adopting the three-in-one equipment from Wuxi Sunray on the 200-ton annual production line of vitamin E succinate, a significant amount of solvent loss was reduced, safety risks were lowered, the level of automation was enhanced, and the number of operators was decreased, generating an annual economic benefit of over 2 million yuan. Due to the closed operation of the equipment, the product quality has been improved, and it occupies a small area. This indicates that the use of the filtration, washing and drying machine has achieved good economic and environmental benefits, and the production is more in line with GMP requirements and standards.

On-site photos of the vitamin raw material drug intermediate refining, purification, filtration, washing and drying machine