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Niacin market and its production technology

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  1) pharmaceutical industry nicotinic acid in the human body has to maintain healthy skin and nerves, promote digestive functions, expansion of blood vessels. Human lack of niacin occurs stomatitis, glossitis, memory loss, depression and colitis symptoms such as abdominal floating. Synthesis of nicotinic acid by intestinal bacteria, can also be generated in vivo tryptophan, generally less prone to a lack of symptoms. However, if the corn and the like without niacin nicotinic acid metabolism of the food or cause food-eating, it will result due to a lack of niacin bark disease. Animals, the lack of niacin, it will because they can not produce enough coenzyme lead to dermatitis, hair removal.


    
Applications in medicine, to nicotinic acid amide tobacco as raw material can be synthesized, Nick kill meters, niacin, inositol tablets, and a series of products off the Spirit ester. Nicotinic acid and ammonia in the synthesis of diethyl Nick kill rice is central stimulant, used to treat central respiratory disease and circulatory failure. Nicotinic acid and the reaction of the corresponding alcohol muscle nicotinic acid ester, ester off spirit, for the treatment of hyperlipidemia, coronary heart disease, migraine, vascular disorders of the slightly such drugs. In recent years, data suggested that nicotinic acid can inhibit the mutagenic effect of anti-swelling medication.

    
(2) feed industry due to animal species. Growth stage, feeding and breeding conditions, differences in the natural acid content in different feed, so the addition of the requirements of nicotinic acid are not the same.

    
(3) The food industry is currently in the food industry in China has not developed the application of nicotinic acid, the amount of very few. According to the Japanese adult 10-20mg daily intake requirements of the Ministry of Health, as the food nutrition fortifier, each kg of niacin in cereal and cereal products allow the addition level 40-50mg. If this requirement can be implemented, the food industry is considerable demand for nicotinic acid.

     
(4) Europe and other developed countries will be other uses for the dye industry nicotinic acid, nicotinic acid triazine reactive dye production, but also for everyday chemicals, such as hair growth promoters, hair color additives, polymer stabilizers, photographic material antioxidants and fog agents, nicotinic acid or a good light additives.

    
l production and demand

    
1.l of foreign production and demand

    
Niacin foreign manufacturers mainly in Western Europe, Japan, Russia, India, Romania and other countries also have production, total global production capacity is about 40,000 t / a. Which have large production company, Switzerland Lonza, the production capacity of about 11,000 t; the German company Degussa annual 6000t. BASF Corporation annual 1500t; Reilly annual output of U.S. 2500t, Nepeya annual output of 2000t; Japan Yurigosei annual output of 2000t; India Indian Drug Companies annual 1000t; Spain Lisa annual output of 1500t and so on.

    
The United States is the world's largest consumer of nicotinic acid, the annual consumption of 1.8 million t, accounting for more than half of global demand, which accounted for 80% of feed additives, food additives and pharmaceuticals accounted for 20%. Western Europe is also a larger consumer area, the annual consumption of about 13,000 t, which accounted for 80% of feed additives. Global niacin consumption of 5% per year growth rate of its production in 2010 is expected to reach 50 000 t.

    
1.2 The domestic production and demand

    
No large-scale production of nicotinic acid manufacturers, usually by the pharmaceutical production, such as the Beijing Second Pharmaceutical Factory, Hebei Pharmaceutical Factory, Shanghai Pharmaceutical Huainan, Guangdong stone squeak pharmaceutical, chemical plant in Changshu, Jiangsu Xinglong and so on. The total output of less than 150Ot, while demand increases every year, to feed, for example, need to feed China in 2001 niacin 2500t, present, China's total demand for nicotinic acid 5000-6000t. Current production can not meet market demand, most dependent on imports, import prices are basically stable at 60,000 -6.5 million / t.

    
Comparison 2 synthesis route

    
2.1 Routing Overview

    
Acid synthesis more, which are summarized as the following line:

    
(L) of potassium permanganate oxidation of nicotinic acid which is the earliest methods of production to 3 - methyl-pyridine as raw material by potassium permanganate oxidation of nicotinic acid. Products slightly red, and inconsistent quality; material 3 - methylpyridine low conversion rate (85%); greater consumption of potassium permanganate (lt 2.5t niacin consumption of potassium permanganate.) The high cost method, equipment corrosion larger, not suitable for industrial production.

    
(2) nitric acid oxidation of nitric acid as oxidant, the mixture of nitric acid solution and pass into the titanium tube MEP reactor, controlling the reaction temperature is 330 ℃, pressure of 29MPa, reaction of 8h, after purified by the separation of nicotinic acid. This method requires a higher temperature, the reaction selectivity, serious equipment corrosion, low yield, waste pollution is serious, color and poor quality products.

     
(3) ozone oxidation method quinoline dissolved in nitric acid solution, the temperature to 40-50 ℃, which leads to ozone formation of ozone quinoline compounds obtained reflux temperature of 2,3 - dipyridyl acid, nicotinic acid and then decarboxylation get. The method is compared with the previous two methods has certain advantages, no equipment corrosion, waste less, low labor intensity, but more expensive ozone, an increase of production costs, the need to build another ozone plant, equipment investment is large, is not suitable large-scale industrial production.

    
(4) gas phase oxidation of gas phase oxidation of air or oxygen-enriched air is the oxidant oxidation of 3 - methyl-pyridine system nicotinic acid. This method was first air Walter alkyl pyridine with the catalyst in the reaction solution, later changed to 3 - methyl-pyridine gasification together with air into the tube reactor, reaction temperature 350-400 ℃, reaction time 3h. Catalyst for the long term applied to oxygen as the oxidant, the oxidation process step can be completed, is a cost-efficient production process. This reaction is the key to select the appropriate catalyst, difficulties still exist, and the reaction temperature is high, yet there are reports of industrialization.

    
(5) electrolytic oxidation is the production of electrolytic oxidation method is widely used as a method of application conditions with mild oxidant is relatively cheap, toxic pollution, less waste, lower production cost advantages, but the electrolysis efficiency of such reactions is low, mainly because the cell membrane permselectivity used in isolation is poor, so that the method for industrial production are more restricted.

    
(6) of the Act hydroxide method of 3 - methylpyridine or MEP as raw materials, and ammonia, by a certain percentage of oxygen in the catalyst under the oxidation reaction to produce smoke nitrile, hydrolysis in alkaline solution and subsequently by the purified nicotinic acid. The reaction carried out under normal pressure or low pressure with high yield, high purity products, safe and reliable product, suitable for continuous large-scale industrial production, industrial preparation of nicotinic acid is widely used abroad, the process route.

    
2.2 nicotinic acid production process abroad

     
(1) Switzerland, Lonza company, India's Indian Drug companies and use pesticide plant in Guangzhou, China 2 - methyl-6 - ethyl-pyridine as the raw material of the process line. It is Lonza's patented technology, the company's production plant scale, well-equipped, technologically advanced, the main equipment to use more anti-corrosion performance, more expensive titanium alloy material. Lonza company formed on the basis of a larger production scale, production cost will be reduced. But for our part, the raw material 2 - methyl -5-- ethyl pyridine must be purchased, making the price higher than that of Lonza niacin companies, and large equipment investment.

    
(2) Another technique is 3 - methyl-pyridine was synthesized by ammonia oxidation of 3 - cyanopyridine, and then by hydrochloric acid hydrolysis of nicotinamide or nicotinic acid. Degussa, Germany and Japan Yurigosei company uses this technology. Materials 3 - picoline pyridine from large-scale production plant by-products, with a wide source of low price, high content of advantages. This method is suitable for our use.

    
3 Progress of domestic technology

     
The current level of production technology of niacin compared with foreign countries there is a considerable gap. Layer filter synthesis Keyuan company, in the original ammonia oxidation, based on the 3 - methyl-pyridine conversion rate of 99%, the yield of nitrile smoke more than 98%, select the appropriate conditions to control the concentration of alkali and reaction temperature by nicotinic acid, smoke up to 99% nitrile conversion. The process is the key to choose the right compound catalyst.

    
Mentioned British Patent GB1317064, a vanadium oxide and titanium dioxide by the molar ratio from 1:0.6:1:32 formed by the mixed oxide catalysts used for ammonia oxidation of pyridine. It was found that highly active catalysts can be prepared to address the shortcomings in the literature. Formula is defined as VaTibZrcOx (the a1; b is 7.5-8; c is 0-0.5; X stands for oxygen atoms required to satisfy the charge balance number), the catalytic component of the preparation steps are as follows: V5 +, Ti4 +, and any kind of solution Zr4 + compounds in water and ammonia solution, precipitation, and then drying the precipitate has the processor and heat into the processor and the catalytic activity by setting steps to form a suitable catalyst components morphology. The appropriate type of titanium is mainly water-soluble components Ti4 + compounds (such as titanium tetrachloride, titanium bromide, titanium nitrate) and organic titanium compounds (such as the four alkyl titanium compounds); appropriate sub-types of units are mainly water-soluble V5 + compounds, such as amine metavanadate; appropriate types of zircon are mainly water-soluble components Zr4 + compounds such as zirconium oxychloride.

    
The catalyst components have been found and produced a mixture of ammonia solution of this precipitation, precipitation generated in this way after the fluid between the pH value of 8-9. Precipitate separated from the first drying, which leads to temperature of 120-140 ℃ in air flow better, and directly release a temperature 360-400 ℃ thermal processor with the presence of air better. Step through a common stereotypes shape of the catalyst with the right. Finally, the catalyst into a temperature between 740-850 ℃ in the presence of air thermal processor, small block, first the formation of the catalyst.

     
Components of the catalyst in the catalytic material can be loaded in the reaction, the reaction conditions in the mobile phase verifiable through its pyridine under high load with high activity, selectivity, long active time. Preferred contact response group was divided into VTi8Ox (where x is as defined before).

    
Experimental production conditions to determine the following: the feed gas by the pyridine, oxygen gas, ammonia and water vapor form, can act as oxygen gas is usually air; if from the 3 - methyl-pyridine nitrile into the smoke, the gas feed from 3 - methylpyridine, air (with oxygen meter), ammonia and water vapor composition, molar ratio 1:7:3:3-1:40:10:45, the preferred ratio range of 1:10 :4:10-1: 30:7:30, the best ratio of 1:12:17:20; the reaction temperature is 200 ℃.

    
3.l Introduction to production technology

     
The 3 - methyl-pyridine, NH3, air and water vapor according to the proportion of 1:4:20:4 feeding, reaction is as follows:



    
Oxidation process carried out in the fluidized bed, the smoke obtained by alkaline nitrile (3%) hydrolysis, and then purified nicotinic acid, the process is as follows:



    
3.2 Technology characteristics

     
The process to 3 - methyl-pyridine conversion rate to 99%, the selectivity tobacco nitrilase increased to 99%. Reaction temperature and pressure greatly reduced. Product yield was increased at the same time, waste pollution under control. 3.3 Product quality standards

    
Products using the technology, quality in line with GB7300-87 requirements, content (dry basis) 99% -101%, melting point 234-238 ℃. Pharmaceutical and other industries to meet the high content of products, high-quality requirements.
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