CN108299600A - A kind of preparation method of Vitamin K3 polymeric material - Google Patents
A kind of preparation method of Vitamin K3 polymeric material Download PDFInfo
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- CN108299600A CN108299600A CN201711299546.1A CN201711299546A CN108299600A CN 108299600 A CN108299600 A CN 108299600A CN 201711299546 A CN201711299546 A CN 201711299546A CN 108299600 A CN108299600 A CN 108299600A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
- C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The present invention relates to a kind of preparation methods of Vitamin K3 polymeric material.It is formed by specified weight number, including butyl acrylate, polyvinyl alcohol, benzoyl peroxide, nano-calcium carbonate, the poly- bonding composition of resin surface, temperature reaction, product obtains Vitamin K3 polymeric material after processing.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, especially a kind of preparation side of Vitamin K3 polymeric material
Method.
Background technology
Vitamin K is the substance for having phylloquinone bioactivity.There are several forms such as K1, K2, K3, K4, wherein K1,
K2 is naturally occurring, is liposoluble vitamin, i.e., the vitamin K1 extracted from green plants and enteric bacteria（Such as large intestine bar
Bacterium）The farnoquinone of synthesis.And K3, K4 are by artificial synthesized, are water-soluble vitamin.Most importantly vitamin K1
And K2.Vitamin K is yellow crystals, and fusing point is 52 DEG C~54 DEG C, not soluble in water usually in oily liquids or solid, can be dissolved in
The organic solvents such as grease and ether.The chemical property of all vitamins K is all relatively stablized, can be acidproof, heat-resisting, in the normal cooking only
Little loss, but it is light sensitive, also easily by alkali and ultraviolet light degradation.Vitamin K reaches nurse most earlier than nineteen twenty-nine by Denmark chemist
It finds and extracts from Animal Liver and flaxseed oil.Vitamin K3 belongs to coagulant, can be used for treating vitamin K deficiency and is drawn
The hemorrhagic disease risen, such as the bad caused vitamin K deficiency of hemorrhage of newborn, intestinal absorption and Hypoprothrombinemia.Dimension
Raw element K3 is mostly white or off-white color crystalline powder, is lumpd after moisture absorption.
CN101347419 discloses a kind of vitamin K, particularly discloses a kind of stable state Vitamin K3 and its preparation side
Method.The stable state Vitamin K3, is characterized in that:It is made of material below:Menadione, sodium pyrosulfite, nicotinoyl
Amine, sulfuric acid.The preparation method of the stable state Vitamin K3 menadione, alcohol water blend is added in 500ML reaction bulbs, fully
Then stirring to pulp adds sodium pyrosulfite, add niacinamide to continue stirring and dissolving, sulfuric acid tune PH=3~5 are then slowly added dropwise, obtain greatly
White crystal is measured, is filtered, washed, dries to obtain K3.
The preparation method and device of a kind of Vitamin K3s of CN103254056B.Method includes by beta-methylnaphthalene stream, oxide
Water-soluble liquid stream and recycle stream combination cooling form reaction liquid stream, persistently to reaction liquid stream cooling reaction formed crude product stream and from
Vitamin K3 is detached in crude product stream；Which part crude product stream reenters reaction liquid stream as recycle stream；Oxide is water-soluble
Liquid stream includes sodium dichromate and sulfuric acid, and CrO3 contents are 200~350g/L, and sulfuric acid content is 400~550g/L, oxide water
The flow-rate ratio of solution stream and beta-methylnaphthalene stream is 7~11:1, beta-methylnaphthalene is 1 with the flow-rate ratio for reacting liquid stream:900~1300；
Temperature control is at 55~65 DEG C when cooling reaction.Device includes blending tank, tubulation retort, separating-purifying component, temperature-controlled member
And flow control component.
The Vitamin K3 product of high-purity is conducive to play better effect, and existing production Vitamin K3 technique is carrying
Pure link is mostly complicated for operation or purifying technique cannot simply produce high-purity Vitamin K3 product, therefore, researches and develops a kind of suitable
For the new adsorbent of Vitamin K3 production, be conducive to the production Vitamin K3 product of more convenient and quicker.
Invention content
The purpose of the present invention is：There is provided a kind of preparation method of Vitamin K3 polymeric material, it is characterised in that prepare step
Suddenly include：
By weight, following components are uniformly mixed, are warming up to 75-95 DEG C, reaction 8-15h is poly- to get being used to Vitamin K3
Condensation material.
Ingredients weight parts
100 parts of butyl acrylate
Poly- bonding composition 8-16 parts of resin surface
0.5-1.5 parts of polyvinyl alcohol
0.5-1 parts of benzoyl peroxide
500-1000 parts of water
25-45 parts of nano-calcium carbonate
By weight, the poly- bonding composition of the resin surface, consisting of：
Ingredients weight parts
100 parts of 1,5- hexadienes
0.1-0.5 parts of 5- methyl rings amyl- 1,3- diene -1,2- diamines
0.01-0.1 parts of 3- ethyoxyls -2- propenoyl isocyanates
0.001-0.01 parts of methylacryoyloxyethyl monomester succinate
0.001-0.01 parts of methylacryoyloxyethyl trimellitic anhydride
0.0001-0.001 parts of 2- aminomethyls-N- allylpyrrolidines
Two (octyl phenol polyoxyethylene) 0.001-0.01 parts of phosphides
The butyl acrylate, polyvinyl alcohol, benzoyl peroxide, nano-calcium carbonate, amyl- diene -1 1,3- of 5- methyl rings,
2- diamines, 3- ethyoxyl -2- propenoyl isocyanates, methylacryoyloxyethyl monomester succinate, methacryloxypropyl second
Base trimellitic anhydride, 2- aminomethyl-N- allylpyrrolidines, two (octyl phenol polyoxyethylene) phosphides are commercial product.
The product of the present invention has the advantages that：
The adsorbent product that the present invention is produced is non-breakable, is easy to detach with product, while heat-resisting endurance is good, not variable
Property；Adsorption rate is fast, and big by the contact area of adsorption production, and the Vitamin K3 product of high-purity can be made.
Specific implementation mode
Following instance is only to further illustrate the present invention, and is not limitation the scope of protection of the invention.
Embodiment 1
Step 1. prepares the poly- bonding composition of resin surface, and every part indicates 1Kg mass, consisting of：
Ingredients weight parts
100 parts of 1,5- hexadienes
0.13 part of the amyl- 1,3- diene -1,2- diamines of 5- methyl rings
0.04 part of 3- ethyoxyl -2- propenoyl isocyanates
0.003 part of methylacryoyloxyethyl monomester succinate
0.005 part of methylacryoyloxyethyl trimellitic anhydride
0.0005 part of 2- aminomethyl-N- allylpyrrolidines
Two (octyl phenol polyoxyethylene) 0.005 part of phosphides
Step 2. prepares adsorbent product, and every part indicates 1Kg mass, consisting of：
Ingredients weight parts
100 parts of butyl acrylate
12 parts of the poly- bonding composition of resin surface
1 part of polyvinyl alcohol
0.75 part of benzoyl peroxide
750 parts of water
35 parts of nano-calcium carbonate
It mixes the above components evenly, is warming up to 85 DEG C, reaction 11.5h is to get to Vitamin K3 polymeric material.
Embodiment 2
Step 1. prepares the poly- bonding composition of resin surface, and every part indicates 1Kg mass, consisting of：
Ingredients weight parts
100 parts of 1,5- hexadienes
0.1 part of the amyl- 1,3- diene -1,2- diamines of 5- methyl rings
0.01 part of 3- ethyoxyl -2- propenoyl isocyanates
0.001 part of methylacryoyloxyethyl monomester succinate
0.001 part of methylacryoyloxyethyl trimellitic anhydride
0.0001 part of 2- aminomethyl-N- allylpyrrolidines
Two (octyl phenol polyoxyethylene) 0.001 part of phosphides
Step 2. prepares adsorbent product, and every part indicates 1Kg mass, consisting of：
Ingredients weight parts
100 parts of butyl acrylate
8 parts of the poly- bonding composition of resin surface
0.5 part of polyvinyl alcohol
0.5 part of benzoyl peroxide
500 parts of water
25 parts of nano-calcium carbonate
It mixes the above components evenly, is warming up to 75 DEG C, reaction 8h is to get to Vitamin K3 polymeric material.
Embodiment 3
Step 1. prepares the poly- bonding composition of resin surface, and every part indicates 1Kg mass, consisting of：
Ingredients weight parts
100 parts of 1,5- hexadienes
0.5 part of the amyl- 1,3- diene -1,2- diamines of 5- methyl rings
0.1 part of 3- ethyoxyl -2- propenoyl isocyanates
0.01 part of methylacryoyloxyethyl monomester succinate
0.01 part of methylacryoyloxyethyl trimellitic anhydride
0.001 part of 2- aminomethyl-N- allylpyrrolidines
Two (octyl phenol polyoxyethylene) 0.01 part of phosphides
Step 2. prepares adsorbent product, and every part indicates 1Kg mass, consisting of：
Ingredients weight parts
100 parts of butyl acrylate
16 parts of the poly- bonding composition of resin surface
1.5 parts of polyvinyl alcohol
1 part of benzoyl peroxide
1000 parts of water
Nano-calcium carbonate Ca45 part
It mixes the above components evenly, is warming up to 95 DEG C, reaction 15h is to get to Vitamin K3 polymeric material.
Comparative example 1
It is added without amyl- 1,3- diene -1, the 2- diamines of 5- methyl rings, other conditions are the same as embodiment 1.
Comparative example 2
3- ethyoxyl -2- propenoyl isocyanates are added without, other conditions are the same as embodiment 1.
Comparative example 3
It is added without methylacryoyloxyethyl monomester succinate, other conditions are the same as embodiment 1.
Comparative example 4
It is added without methylacryoyloxyethyl trimellitic anhydride, other conditions are the same as embodiment 1.
Comparative example 5
2- aminomethyl-N- allylpyrrolidines are added without, other conditions are the same as embodiment 1.
Comparative example 6
Two (octyl phenol polyoxyethylene) phosphides are added without, other conditions are the same as embodiment 1.
Embodiment 4
The Vitamin K3 crude product that mass percent concentration is about 50% is passed through equipped with 500g embodiments 1-3 and comparative example 1-6 dimensions
The 1000L exchange columns of raw element K3 polymeric materials, temperature 60 C, flow velocity 0.5BV/h, under the conditions of absorption purify, use gas-chromatography
The mass percentage for detecting efflux, is shown in Table 1.
Table 1：Vitamin K3 product purity after the adsorbent product absorption that different process is produced.
Claims (3)
1. a kind of preparation method of Vitamin K3 polymeric material, it is characterised in that group becomes by weight：
Ingredients weight parts
100 parts of butyl acrylate
Poly- bonding composition 8-16 parts of resin surface
0.5-1.5 parts of polyvinyl alcohol
0.5-1 parts of benzoyl peroxide
500-1000 parts of water
25-45 parts of nano-calcium carbonate.
2. a kind of preparation method of Vitamin K3 polymeric material according to claim 1, it is characterised in that by weight,
The resin surface polymerized monomer mixed liquor group becomes：
Ingredients weight parts
100 parts of 1,5- hexadienes
0.1-0.5 parts of 5- methyl rings amyl- 1,3- diene -1,2- diamines
0.01-0.1 parts of 3- ethyoxyls -2- propenoyl isocyanates
0.001-0.01 parts of methylacryoyloxyethyl monomester succinate
0.001-0.01 parts of methylacryoyloxyethyl trimellitic anhydride
0.0001-0.001 parts of 2- aminomethyls-N- allylpyrrolidines
Two (octyl phenol polyoxyethylene) 0.001-0.01 parts of phosphides.
3. a kind of preparation method of Vitamin K3 polymeric material according to claim 1, it is characterised in that preparation method
For：It mixes the above components evenly, is warming up to 75-95 DEG C, reaction 8-15h is to get to Vitamin K3 polymeric material.
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| CN201711299546.1A CN108299600A (en) | 2017-12-09 | 2017-12-09 | A kind of preparation method of Vitamin K3 polymeric material |
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| CN201711299546.1A CN108299600A (en) | 2017-12-09 | 2017-12-09 | A kind of preparation method of Vitamin K3 polymeric material |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774286A (en) * | 2015-04-07 | 2015-07-15 | 浙江大学 | Preparation method of polyacrylate macroporous cross-linked polymer and product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774286A (en) * | 2015-04-07 | 2015-07-15 | 浙江大学 | Preparation method of polyacrylate macroporous cross-linked polymer and product |
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