Mixing-drying reactor for the synthesis of plant protection active ingredients
A plant protection product has been fully formulated. The active ingredients are coated multiple times. This ensures that the release of the active ingredients is controlled.
Plant protection products are marketed as formulated end products. The active ingredients are often coated multiple times. This allows the release of the active ingredients to be precisely controlled.
Powdered active ingredients offer process engineering advantages. They are transported without any water content. This reduces volume and costs. Storage is space-saving and does not require refrigeration. Shelf life is long under suitable conditions. Sub-quantities can be precisely metered. Good instant properties enable rapid further processing at the point of use.
Vacuum mixing and drying is a gentle separation process. Liquids evaporate at reduced pressure and low temperatures. This protects temperature-sensitive substances. During drying, viscoelastic states may occur. Lumps and agglomerates form. As the vacuum drying progresses, these disintegrate completely. The result is a homogeneous, free-flowing powder.
- Question: What happens in the vacuum mixing-drying synthesis reactor during the synthesis of active pharmaceutical ingredients? Short answer: Solids, reagents and liquids are mixed intensively. The reaction takes place at a specified temperature and pressure. Following chemical precipitation or crystallisation and washing, a vacuum is applied. This lowers the boiling point, allowing the solvents to evaporate at a lower temperature. They are recovered in the condenser. In the amixon® unit, the processes run particularly efficiently. Three-dimensional mixing takes place despite changes in the rheology of the synthesis product. At the end of the process, a dry, free-flowing powder is produced.
- Question: What characterises a particularly high-performance, multi-purpose synthesis plant? Short answer: It can be adapted to a wide variety of synthesis steps without the need for major modifications.
- Question: How do synthetically produced products behave when dried in a vacuum contact dryer? Short answer: They undergo various rheological states – from a pumpable suspension to a dry, free-flowing powder. When amixon® units are used, the particle size distribution of the synthetically produced powder is largely preserved. The powder is low in dust or dust-free.
- Question: How does a vacuum mixing-drying synthesis reactor ensure the production of high-purity products? What design and process engineering measures ensure contamination-free operation and protect the environment? Short answer: This is achieved by a) a pressure-resistant and gas-tight mixing chamber. b) It is easy to clean. It also features c) high-quality flange and shaft seals. d) Gas-tight feed and discharge fittings prevent contamination. e) Corrosion-resistant materials ensure high-purity active ingredient formulations. f) amixon® units are designed to comply with GMP and FDA standards.
- Question: How can a process equipment manufacturer support the plant operator throughout the entire life cycle of the plant? Short answer from amixon®: 1). Through custom-designed process equipment. 2). Through test centres available worldwide for scale-up tests and 3). Through a global service concept. 4). Through a global service concept and 5). Through training the operator to carry out maintenance independently.
1) Mixing, Blending, Reacting, vacuum drying, powder formulation
When synthesising active ingredients, the consistencies of the reaction products often change. It does not matter whether they are active pharmaceutical ingredients (APIs) or pesticides. Consistency changes often occur even after the synthesis reactions have been completed. Vacuum mix drying turns pumpable suspensions into free-flowing powders. Synthesis plants are generally used as multi-purpose plants for various synthesis steps and must work reliably regardless of the rheological properties of the starting materials and products.
This requirement is met by a new amixon® vacuum mixing dryer/synthesis reactor, which was developed for a well-known manufacturer of active ingredients. The system can process solids with a dusty, flaky and powdery consistency. The same system can also process pasty, sludgy and viscous products.
When synthesising active ingredients, the consistencies of the reaction products often change. It does not matter whether they are active pharmaceutical ingredients (APIs) or pesticides. Consistency changes often occur even after the synthesis reactions have been completed. Vacuum mix drying turns pumpable suspensions into free-flowing powders. Synthesis plants are generally used as multi-purpose plants for various synthesis steps and must work reliably regardless of the rheological properties of the starting materials and products.
This requirement is met by a new amixon® vacuum mixing dryer/synthesis reactor, which was developed for a well-known manufacturer of active ingredients. The system can process solids with a dusty, flaky and powdery consistency. The same system can also process pasty, sludgy and viscous products.
2) Plant diagram
This synthesis route produces active ingredients. The solvents used are largely recovered. The end product is a powdery solid. This is then ‘diluted’ in another plant and ‘formulated’ in such a way that it is safe and convenient for the end user.
This synthesis route produces active ingredients. The solvents used are largely recovered. The end product is a powdery solid. This is then ‘diluted’ in another plant and ‘formulated’ in such a way that it is safe and convenient for the end user.
3) Pumpable, lumpy, crumbly, powdery
During vacuum drying, the rheological properties of the product change. The decrease in the liquid content changes the product:
- Initially, a pumpable suspension is present.
- This becomes a lumpy paste.
- Then the product becomes crumbly.
- When dry, the product is a fine powder.
Even in multi-stage synthesis processes, the first stage begins with the dissolution of the powdery base chemical in a suitable liquid template and ends with a drying process in a vacuum contact dryer. At the end of each synthesis, the liquid is crystallised. This is followed by several washing processes. Finally, the centrifuge-damp crystal mixture must be gently dried. The granular structure of the bulk material should be retained, as dust particles are undesirable.
amixon® process equipment also achieves an ideal mixing result when it is operated particularly slowly. Even then, good heat transfer takes place. Low speeds result in a particularly gentle mixing and drying process. If required, intensive deagglomeration can also be carried out with the same machine.
Particularly high vacuums allow liquids to be vaporised at low temperatures. This is always an advantage when the active ingredients are temperature-sensitive.
During vacuum drying, the rheological properties of the product change. The decrease in the liquid content changes the product:
- Initially, a pumpable suspension is present.
- This becomes a lumpy paste.
- Then the product becomes crumbly.
- When dry, the product is a fine powder.
Even in multi-stage synthesis processes, the first stage begins with the dissolution of the powdery base chemical in a suitable liquid template and ends with a drying process in a vacuum contact dryer. At the end of each synthesis, the liquid is crystallised. This is followed by several washing processes. Finally, the centrifuge-damp crystal mixture must be gently dried. The granular structure of the bulk material should be retained, as dust particles are undesirable.
amixon® process equipment also achieves an ideal mixing result when it is operated particularly slowly. Even then, good heat transfer takes place. Low speeds result in a particularly gentle mixing and drying process. If required, intensive deagglomeration can also be carried out with the same machine.
Particularly high vacuums allow liquids to be vaporised at low temperatures. This is always an advantage when the active ingredients are temperature-sensitive.
4) Highly pure and gas-tight
If further powdered components are to be added to the dry product before filling, this is done in the same apparatus. A mixing tool with a helical outer contour rotates in the centre of the conical-cylindrical mixing chamber. This conveys the products upwards along the container wall; once at the top, the products flow downwards in the centre. The mixer-dryer reactor delivers ideal mixes at filling levels of approx. 15 to 100 %. The container is emptied completely using the patented SinConvex® mixing tool.
The vacuum mixing dryer is capable of producing high-purity active ingredient preparations. The mixing tool is only driven from above and is fully heatable.
The shaft seals of the mixer shaft and the cutting rotor are designed as mechanical seals and are gas-tight. The dead space-free shut-off valve at the end of the mixing cone is also particularly gas-tight.
The mixing chamber of the reactor is made of Hastelloy C 22. This material has high strength and is also particularly resistant to corrosion. The entire system complies with the principles of ‘Good Manufacturing Practice’ (GMP) and the requirements of the FDA. All qualification steps are carried out in accordance with GMP. The complete documentation of development, production and commissioning also fulfils the high requirements of the pharmaceutical industry. amixon® has produced numerous mixing-drying reactors for chemical and pharmaceutical applications with container sizes from 1 to 25,000 litres. The range extends to small and large vacuum mixing dryers/synthesis reactors.
If further powdered components are to be added to the dry product before filling, this is done in the same apparatus. A mixing tool with a helical outer contour rotates in the centre of the conical-cylindrical mixing chamber. This conveys the products upwards along the container wall; once at the top, the products flow downwards in the centre. The mixer-dryer reactor delivers ideal mixes at filling levels of approx. 15 to 100 %. The container is emptied completely using the patented SinConvex® mixing tool.
The vacuum mixing dryer is capable of producing high-purity active ingredient preparations. The mixing tool is only driven from above and is fully heatable.
The shaft seals of the mixer shaft and the cutting rotor are designed as mechanical seals and are gas-tight. The dead space-free shut-off valve at the end of the mixing cone is also particularly gas-tight.
The mixing chamber of the reactor is made of Hastelloy C 22. This material has high strength and is also particularly resistant to corrosion. The entire system complies with the principles of ‘Good Manufacturing Practice’ (GMP) and the requirements of the FDA. All qualification steps are carried out in accordance with GMP. The complete documentation of development, production and commissioning also fulfils the high requirements of the pharmaceutical industry. amixon® has produced numerous mixing-drying reactors for chemical and pharmaceutical applications with container sizes from 1 to 25,000 litres. The range extends to small and large vacuum mixing dryers/synthesis reactors.
5) amixon® process equipment is always customised to meet individual customer requirements
The requirements for a processing mixer are always individual. amixon® has more than 30 test mixers for process testing in the technical centres in Paderborn. Further test machines are located in Memphis (USA), Osaka (Japan), Bangkok (Thailand), Tianjin (China) and Satara (India).
As a contract manufacturer, amixon® realises customer requirements down to the last detail. 140 employees realise a considerable vertical range of manufacture at the only production site in Paderborn. The after-sales service team is responsible for the maintenance and inspection of the systems after commissioning.
The ‘amixon® Excellent Service’ is a worldwide concept with bases in Paderborn, Memphis, Osaka and Bangkok. In addition to offering ‘lifelong’ equipment support, service employees as well as operators and developers are trained to carry out inspections and maintenance themselves.
Plant protection products (Part 1)
Plant protection products (Part 2)
The requirements for a processing mixer are always individual. amixon® has more than 30 test mixers for process testing in the technical centres in Paderborn. Further test machines are located in Memphis (USA), Osaka (Japan), Bangkok (Thailand), Tianjin (China) and Satara (India).
As a contract manufacturer, amixon® realises customer requirements down to the last detail. 140 employees realise a considerable vertical range of manufacture at the only production site in Paderborn. The after-sales service team is responsible for the maintenance and inspection of the systems after commissioning.
The ‘amixon® Excellent Service’ is a worldwide concept with bases in Paderborn, Memphis, Osaka and Bangkok. In addition to offering ‘lifelong’ equipment support, service employees as well as operators and developers are trained to carry out inspections and maintenance themselves.
Plant protection products (Part 1)
Plant protection products (Part 2)
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