N-valeric acid is a short-chain saturated fatty acid, also known as valeric acid, valerenic acid, and oxalic acid. Valeric acid is a colorless transparent liquid at room temperature, with a relative density of 0.9391.It is flammable and has an unpleasant smell of stinky socks. It exists in the perennial flowering plant Valeriana officinalis.
Valeric Acid Property
110-111 °C10 mm Hg(lit.)
0.939 g/mL at 25 °C(lit.)
3.5 (vs air)
0.15 mm Hg ( 20 °C)
Store below +30°C.
Clear colorless to pale yellow
3.95(1 mM solution);3.43(10 mM solution);2.92(100 mM solution);
at 1.00 % in propylene glycol. sickening putrid acidic sweaty rancid
40 g/L (20 ºC)
Valeric Acid Uses
Valeric Acid is a crucial chemical basic material, generally used for the synthesis of valeric acid esters, valeric acid esters are volatile and have a pleasant scent, and also can be made use of in fragrances as well as cosmetics. Ethyl valerate and pentyl valerate have fruit Scent, utilized as a preservative. Valerate is widely made use of in seasonings, medicine, lubricants, plasticizers as well as other sectors, and is a commonly utilized chemical raw material.
Valeric Acid is used in the manufacturing of polyol esters of cooling agents (CFC replaces), artificial lubricating substances for electrical motors and also jet engines, esterified with lower alcohols as solvents and as scents and also perfumes, and can likewise be utilized in the production of crop security products.
Production Method of Valeric Acid
In order to solve the problems in the prior art, an embodiment of the present invention provides a method for producing Valeric Acid. Described technical scheme is as follows:
On the one hand, a kind of method of producing Valeric Acid is provided, is characterized in that, comprises the following steps:
(1) Preparation of Grignard reagent: add a part of 1-chlorobutane to the mixture of metal magnesium and solvent, after heating to initiate the reaction, add the remaining 1-chlorobutane dropwise within 3~10min, and keep the reaction system at reflux state, after the 1-chlorobutane has been added dropwise, the reaction system is continued to reflux until the reaction is completed, wherein the mol ratio of 1-chlorobutane to magnesium is (1~20):9, the 1-chlorobutane added in the first part Alkanes are (22~24)% of the total amount of 1-chlorobutane, the solvent is tetrahydrofuran or ether, and the volume ratio of solvent to 1-chlorobutane is (4~5): 1;
(2) Add the reaction mixture obtained in (1) dropwise to a reaction vessel equipped with dry ice within 10~30min. After the dropwise addition, naturally rise to room temperature, then add MHSO4, stir, and suction filter after the reaction is complete, and the filtrate is acidified Rear purification obtains n-valeric acid, wherein the magnesium added in (1): the dry ice added in (2): MHS04=9:27:7, M is K or Na.
Preferably, in the step (1), the 1-chlorobutane added in the first part is 23% of the total amount of 1-chlorobutane.
Preferably, in the step (1), the molar ratio of 1-chlorobutane to magnesium is 1: (1.4~1.6), more preferably 2: 3.
Preferably, the step (1) is carried out under the protection of an inert gas. Because the Grignard reagent will be consumed by air and water, such as nitrogen or argon, which will affect the reaction effect.
Preferably, in the step (2), the purification refers to acidifying the filtrate to a pH value of (3~4), then extracting the acidified filtrate with ether, merging and drying the organic phases, and finally removing the ether to obtain The Valeric Acid. Usually, the reagent added during acidification is 2mol/L dilute hydrochloric acid or 1mol/L dilute sulfuric acid.
More preferably, said M is K.
More preferably, the solvent is tetrahydrofuran.
In the described step (1), a part of 1-chlorobutane added earlier can be used as an initiator to initiate the reaction. After the reaction is initiated, it will exotherm, so that the reaction system boils, and the solvent begins to reflux. As a known technology, proper heating is required during the initiating reaction to promote the initiation of the initiating reaction. Then the remaining 1-chlorobutane can be added dropwise in 3~10min (preferably 4~6min, such as 5 minutes). If the reaction is violent, the rate of addition should be properly controlled to maintain the reaction system in a reflux state. Obviously, this step reaction temperature is relevant with the boiling point of concrete solvent, when solvent adopts tetrahydrofuran, the reaction temperature of step (1) is controlled at 25 DEG C～reflux temperature, promptly before dripping remaining 1-chlorobutane, reaction temperature is in 25°C～reflux temperature, after the remaining 1-chlorobutane is added dropwise, the reaction temperature is basically stable at the reflux temperature. After dropping the remaining 1-chlorobutane, the required reaction time can be determined experimentally by those skilled in the art, preferably 1 ~ 3h, such as 2h.
In the step (2), the reaction mixture obtained by (1) is added dropwise in a reaction vessel equipped with dry ice within 10 ~ 30min, for example, the time for adding is 30 minutes.
As common knowledge in the field, the preparation of Grignard reagent needs to be carried out under anhydrous conditions, so the reaction raw materials must be anhydrous, and water removal treatment can be used in advance. For example, 1-chlorobutane is put into the reaction after freezing and deicing.
Specific Implementation of Valeric Acid
The three-necked round-bottom flask is equipped with a stirring device, a reflux condenser, a constant pressure dropping funnel, and a % protection device. Add Mg (2.16g, 90mmol) and dry THF (30mL) to the three-necked flask. 1-Chlorobutane (1.5 mL) was added to the system, followed by heating to initiate the reaction. After the initiation was successful, the remaining 1-chlorobutane (5.0 mL) was added dropwise to the system within 5 minutes to maintain the reaction system in a reflux state. After the 1-chlorobutane was added dropwise, heating made the reaction system continue to reflux for 2 hours, and the prepared butyl Grignard reagent was directly used in the next step reaction without purification.
The two-necked round bottom bottle is equipped with a stirring device, a constant pressure dropping funnel, and a N2 protection device. Add dry ice (270mmol) in the two-necked flask, and slowly dropwise add the above-mentioned prepared butyl Grignard reagent therein. After the dropwise addition was completed in 30 minutes, it was naturally warmed up to room temperature, then KHS04 (90mmol) was added to the system, stirred for about 30 minutes and then suction filtered. The filtrate was acidified with 2mo 1/L dilute hydrochloric acid to adjust the pH=3-4, and then the product was extracted with ether until complete. The extracts were combined and dried with a desiccant, filtered to remove the desiccant, concentrated and evaporated to diethyl ether to obtain pure Valeric Acid with a yield of 85%.
About Products: If you need Valeric Acid, the cosmetic raw material, please contact our service staff directly, we will provide you with high-quality products at the best price. As an experienced Valeric Acid manufacturer and supplier, ZSpharmac will provide Valeric Acid raw materials to customers all over the world for a long time. Over the years, the company has been adhering to the spirit of “integrity management, strict quality control, customer first”, and has won unanimous praise from domestic and foreign customers.
Company Profile and Corporate Culture
ZhiShang Chemical is owned by ZhiShang Group is a professional new-type chemicals enterprise combined into research and development, production and sales .
The company’s competitive product is pharmaceutical raw materials and intermediates (especially carbohydrate derivatives Series), In recent years, the company has made a major breakthrough in food and feed additives, plant extraction, industrial chemicals industry .
The company insists on the spirit of “sincere management, strict quality control, customer as god” , get consistent high praise from customers at home and abroad.
OUR MISSION Help China Chemicals to benefit the happiness of human life OUR VISSION Become the most trusted chemical supplier in the world OUR BUSINESS PHILOSOPHY Striver – oriented, enrich employees, customer first, deep service, seek development OUR VALUES Be prepared for danger in times of peace, forge ahead actively, unity and cooperation, and be brave to fight
The production base is located in Zhangqiu chemical industry park and Tai’an high-tech chemical industry park. laboratory and workshop in strict accordance with the GMP standard and the product fit national ISO9001 and ISO2000 standards.
“Zhishang” products are exported to Europe, North and South America, the Middle East, Asia Pacific and Africa area, so as to establish a long-term and stable cooperation relationship with customer in the world.
Business Type: Manufacturer
Product Range: Cosmetic raw materials
Products/Service:Cosmetic raw materials (flavors and fragrances,antioxidant products, moisturizing and hydrating, whitening agents, cosmetic additives)
Factory Location : Diao Town Industry Park, Zhangqiu City, Jinan City, Shandong Province, China.
* Prompt reply and 24 hours online, professional team to provide best price and high quality product.
* Sample testing support.
* Every batch of products will be tested to ensureits quality.
*The packing also can be according the customers` requirment.
*Any inquiries will be replied within 24 hours.
*we provide Commerical Invoice, Packing List, Bill of loading, COA , Health certificate and Origin certificate. If your markets have any special requirements, let us know.
*The fact of logistics information monitoring.
* Any questions about the product can be consulted at any time.
*Product has any problem can return.
Do you accept sample order?
We will make samples before mass production, and after sample approved, we’ll begin mass production. Doing 100% inspection during production, then do random inspection before packing.
HOW TO CONFIRM THE PRODUCT QUALITY BEFORE PLACING ORDERS?
You can get free samples for some products,you only need to pay the shipping cost or arrange a courier to us and take the samples. You can send us your product specifications and requests,we will manufacture the products according to your requests.
What’s your MOQ?
Our MOQ is 1kg. But usually we accept less quantity such as 100g on the condition that sample charge is 100% paid.
Do you supply product report?
Yes. We’ll give you product analysis report before shipping.
Is there a discount?
Different quantity has different discount.
1. ≤50kg, Express delivery recommended, usually called as DDU service;
2. ≤500kg, Air shipping recommended, usually called as FOB, CFR, or CIF service;
3. >500kg, sea shipping recommended, usually called as FOB, CFR, or CIF service;
4. For high value products, please select air shipping and express delivery for safe.