CN107954855A - A kind of preparation method of beta-hydroxy-Beta-methyl calcium butyrate - Google Patents

A kind of preparation method of beta-hydroxy-Beta-methyl calcium butyrate Download PDF

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Publication number
CN107954855A
CN107954855A CN201711166893.7A CN201711166893A CN107954855A CN 107954855 A CN107954855 A CN 107954855A CN 201711166893 A CN201711166893 A CN 201711166893A CN 107954855 A CN107954855 A CN 107954855A
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China
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beta
hydroxy
methyl
preparation
calcium butyrate
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CN201711166893.7A
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Chinese (zh)
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汤素葵
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Jinhu Shenkai Industrial Co Ltd
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Jinhu Shenkai Industrial Co Ltd
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Priority to CN201711166893.7A priority Critical patent/CN107954855A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/16Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
    • C07C51/285Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with peroxy-compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Disintegrating Or Milling (AREA)

Abstract

The invention discloses a kind of preparation method of β hydroxyls β methylbutanoic acid calcium, including, sulfuric acid, glacial acetic acid, hydrogen peroxide are mixed, Peracetic acid is collected in an isothermal reaction, distillation;The Peracetic acid is mixed with diacetone alcohol, adds methyl acetate, secondary isothermal reaction, β hydroxyl β methylbutanoic acids are collected in distillation;Add water to the β hydroxyls β methylbutanoic acids, after adjusting pH value of solution, dissolve by heating filtering, take filtrate to add calcium chloride, stirring reaction, adjusts pH, separates out β hydroxyl β methylbutanoic acid calcium, filtering, drying, obtains β hydroxyl β methylbutanoic acid calcium, carries out ultramicro grinding and obtains product.β hydroxyls β methylbutanoic acid calcium high incomes produced by the present invention, synthetic method high-efficiency environment friendly, meets the synthesis theory of Green Chemistry, has a vast market prospect.

Description

A kind of preparation method of beta-hydroxy-Beta-methyl calcium butyrate
Technical field
The invention belongs to nutrition fortifier technical field, and in particular to a kind of preparation side of beta-hydroxy-Beta-methyl calcium butyrate Method.
Background technology
Beta-hydroxy-Beta-methyl butyric acid (β-Hydroxy- β-Methyl Butyrate, HMB, molecular formula C5H10O3) it is required The mesostate of amino acid leucine.Leucine is branched-chain amino acid, belongs to essential amino acid, cannot produce in vivo, right Health is particularly significant, and the mankind must ensure the intake of leucine by diet, and HMB is the intermediate supersession production of leucine Thing.Contain HMB in food, human body itself can also produce a small amount of HMB.At present health-product market sale be HMB calcium salts Single carbohydrate, is often beta-hydroxy-Beta-methyl calcium butyrate.Although it is not yet clear and definite in the metabolic mechanism of human body, it has been proposed For to the muscle protein breakdown in resistive exercise, helping promote to greatest extent the growth of muscle volume.There is research Person proposes hypothesis:HMB may be exactly the required constituent of muscle cell membrane under exercise stress state;Or its may adjust it is some The enzymatic activity to play an important role to muscle growth.Zoopery including poultry, ox, pig is shown:Supplement HMB can increase thin Weight, reduce body fat.
The prior art is prepared in beta-hydroxy-Beta-methyl calcium butyrate, however it remains high cost, poor efficiency, has asking for pollution Topic, does not meet the theory of Green Chemistry, it is difficult to which large-scale promotion produces.
The content of the invention
The purpose of this part is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferably to implement Example.It may do a little simplified or be omitted to avoid our department is made in this part and the description of the present application summary and denomination of invention Point, the purpose of specification digest and denomination of invention obscure, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of the technological gap of the preparation method of above-mentioned and/or existing beta-hydroxy-Beta-methyl calcium butyrate, it is proposed that this hair It is bright.
It is therefore an object of the present invention to solve deficiency of the prior art, there is provided a kind of beta-hydroxy-Beta-methyl calcium butyrate Preparation method.
In order to solve the above technical problems, the present invention provides following technical solution:A kind of preparation method of feed addictive, Including sulfuric acid, glacial acetic acid, hydrogen peroxide being mixed, Peracetic acid is collected in an isothermal reaction, distillation;By the Peracetic acid Mixed with diacetone alcohol, add methyl acetate, secondary isothermal reaction, beta-hydroxy-Beta-methyl butyric acid is collected in distillation;To the β-hydroxyl Base-Beta-methyl butyric acid adds water, after adjusting pH value of solution, dissolves by heating filtering, takes filtrate to add calcium chloride, and stirring reaction, adjusts pH, Beta-hydroxy-Beta-methyl calcium butyrate is separated out, is filtered, drying, obtains beta-hydroxy-Beta-methyl calcium butyrate, carries out ultramicro grinding and is produced Product..
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:Described one Secondary isothermal reaction, its be temperature be 40~50 DEG C, mixing speed be 200~250rpm, reaction 8~12min.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:Described two Secondary isothermal reaction, its be temperature be 25~35 DEG C, mixing speed be 80~120rpm, reaction 50~70min.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:It is described to stir Reaction is mixed, it is 20~30min of stirring reaction under 350~450rpm.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:The tune Save pH value of solution, its be by solution adjust to pH be 5.8~6.2.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:The tune PH is saved, it is that pH is adjusted most 6.3~6.7.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:The sulphur Sour mass concentration is 8~15%, and the volume ratio of itself and glacial acetic acid is 1:8~10.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:The mistake Hydrogen oxide mass concentration is 25~35%, and the volume ratio of itself and glacial acetic acid is 2.5~3.5:1.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:The steaming Collection Peracetic acid is evaporated, it is that the cut of 60 DEG C of vacuum distillation collection obtains Peracetic acid.
As a kind of preferred solution of the preparation method of beta-hydroxy of the present invention-Beta-methyl calcium butyrate, wherein:The steaming Collection beta-hydroxy-Beta-methyl butyric acid is evaporated, it is that the cut of 70 DEG C of distillation collection obtains methyl acetate, and the material after distillation is β-hydroxyl Base-Beta-methyl butyric acid solution.
Beneficial effect possessed by the present invention:
Beta-hydroxy produced by the present invention-Beta-methyl calcium butyrate reaction is gentle, and high income, synthetic method high-efficiency environment friendly, meets The synthesis theory of Green Chemistry, has a vast market prospect.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this For the those of ordinary skill of field, without having to pay creative labor, it can also be obtained according to these attached drawings other Attached drawing.Wherein:
Fig. 1 is the disintegrating apparatus overall structure diagram arrived involved in embodiment 1~3;
Fig. 2 is the connection unit structure diagram arrived involved in embodiment 4;
Fig. 3 is the dust removing units structure diagram arrived involved in embodiment 4;
Fig. 4 is the collector unit structure diagram arrived involved in embodiment 4;
Fig. 5 is the pulverizing unit structure diagram arrived involved in embodiment 4;
Fig. 6 is the control unit structure diagram arrived involved in embodiment 4;
Fig. 7 is the dust part structure diagram arrived involved in embodiment 4;
Fig. 8 is the driving part structure diagram arrived involved in embodiment 4;
Fig. 9 is the first external member partial structurtes enlarged diagram arrived involved in embodiment 5;
Figure 10 is the second external member partial structurtes enlarged diagram arrived involved in embodiment 5;
Figure 11 is the connecting pipe port organization schematic diagram arrived involved in embodiment 5;
Figure 12 is the locking piece partial structurtes enlarged diagram arrived involved in embodiment 5;
Figure 13 is that the locking piece arrived involved in embodiment 5 installs close-up schematic view;
Figure 14 is the adjusting part structure diagram arrived involved in embodiment 6;
Figure 15 is the first counterpart structure diagram arrived involved in embodiment 6;
Figure 16 is the second counterpart structure diagram arrived involved in embodiment 6;
Figure 17 is the rebound part structure diagram arrived involved in embodiment 6.
Embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to specific embodiment pair The embodiment of the present invention is described in detail.
Many details are elaborated in the following description to facilitate a thorough understanding of the present invention, still the present invention can be with Implemented using other different from other manner described here, those skilled in the art can be without prejudice to intension of the present invention In the case of do similar popularization, therefore the present invention is from the limitation of following public specific embodiment.
Secondly, " one embodiment " or " embodiment " referred to herein refers to may be included at least one realization side of the present invention A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to Same embodiment, nor the single or selective embodiment mutually exclusive with other embodiment.
Embodiment 1
It is 30% by sulfuric acid solution and 2000ml glacial acetic acid, 6000ml mass concentrations that 200ml mass concentrations are 10% Hydrogen peroxide mixes, and 10min is reacted at 45 DEG C, and mixing speed is 200rpm therebetween, and 60 are collected by being evaporated under reduced pressure after reaction DEG C cut, obtain peroxide acetate aqueous solution 2500ml, it mixed with the diacetone alcohol of 1250ml, add 2000ml acetic acid first Ester, reacts 1h at 30 DEG C, and mixing speed is 100rpm therebetween, and 70 DEG C of cut is collected in distillation, methyl acetate is obtained, after distillation Material be beta-hydroxy-Beta-methyl butyric acid solution, thereto plus water 2500ml, then add sodium hydroxide solution and adjust to pH and is 6.0, filter after heating for dissolving, take filtrate to add 1000g calcium chloride.Stirring reaction 20min, adds sodium hydroxide under 400rpm It is 6.5 to adjust to pH, separates out beta-hydroxy-Beta-methyl calcium butyrate, filters, and drying, obtains beta-hydroxy-Beta-methyl calcium butyrate 1704g, Feed system 600 is put into, is crushed into crushing system 500, is then received by cyclone collector 400, deduster 300 Collection, obtains the small product of particle diameter.Final products average grain diameter is 1.4 μm, and particle size range is 0.7~3.5 μm.
Embodiment 2
It is 30% by sulfuric acid solution and 1800ml glacial acetic acid, 5400ml mass concentrations that 200ml mass concentrations are 10% Hydrogen peroxide mixes, and 12min is reacted at 50 DEG C, and mixing speed is 250rpm therebetween, and 60 are collected by being evaporated under reduced pressure after reaction DEG C cut, obtain peroxide acetate aqueous solution 1900ml, it mixed with the diacetone alcohol of 1100ml, add 2000ml acetic acid first Ester, reacts 70min at 35 DEG C, and mixing speed is 120rpm therebetween, and 70 DEG C of cut is collected in distillation, obtains methyl acetate, steams Material after evaporating is beta-hydroxy-Beta-methyl butyric acid solution, thereto plus water 2100ml, then add sodium hydroxide solution adjust to PH is 6.0, is filtered after heating for dissolving, takes filtrate to add 1000g calcium chloride.Stirring reaction 30min at 450 rpm, adds hydrogen-oxygen It is 6.5 to change sodium to adjust to pH, separates out beta-hydroxy-Beta-methyl calcium butyrate, filters, drying, obtains beta-hydroxy-Beta-methyl calcium butyrate 1690g, is put into feed system 600, is crushed into crushing system 500, is then passed through cyclone collector 400, dedusting Device 300 is collected, and obtains the small product of particle diameter.Final products average grain diameter is 1.3 μm, and particle size range is 0.8~3.8 μm.
Embodiment 3
It is 30% by sulfuric acid solution and 2000ml glacial acetic acid, 5000ml mass concentrations that 200ml mass concentrations are 10% Hydrogen peroxide mixes, and 10min is reacted at 40 DEG C, and mixing speed is 200rpm therebetween, and 60 are collected by being evaporated under reduced pressure after reaction DEG C cut, obtain peroxide acetate aqueous solution 1800ml, it mixed with the diacetone alcohol of 900ml, add 1600ml acetic acid first Ester, reacts 50min at 25 DEG C, and mixing speed is 120rpm therebetween, and 70 DEG C of cut is collected in distillation, obtains methyl acetate, steams Material after evaporating is beta-hydroxy-Beta-methyl butyric acid solution, thereto plus water 2300ml, then add sodium hydroxide solution adjust to PH is 6.0, is filtered after heating for dissolving, takes filtrate to add 1000g calcium chloride.Stirring reaction 30min, adds hydrogen-oxygen under 350rpm It is 6.5 to change sodium to adjust to pH, separates out beta-hydroxy-Beta-methyl calcium butyrate, filters, drying, obtains beta-hydroxy-Beta-methyl calcium butyrate 1650g, is put into feed system 600, is crushed into crushing system 500, is then passed through cyclone collector 400, dedusting Device 300 is collected, and obtains the small product of particle diameter.Final products average grain diameter is 1.6 μm, and particle size range is 0.4~4.6 μm.
Embodiment 4
Micronizer involved in embodiment 1~3, such as Fig. 1, its agent structure mainly include five component units, respectively For connection unit 100, dust removing units 200, collector unit 300, pulverizing unit 400 and control unit 500.
As shown in Fig. 2~8, connection unit 100 includes the first external member 101,102 and second external member 103 of locking piece, first set 101 and second external member 103 of part is connected by locking piece 102, it is particularly located at dust removing units 200 and collector unit 300 Between, and between collector unit 300 and pulverizing unit 400, provide the foundation for being fastenedly connected for three;Dust removing units 200 Including air inducing part 201 and dust part 202, both can form a complete dust removing units 200, and air inducing part 201 and dust part Connected between 202 by connection unit 100;Collector unit 300 includes collection grain part 301 and separation member 302;Pulverizing unit 400 wraps Include inlet 401 and actuator 402;Control unit 500 includes regulation and control panel 501 and cabinet 502, and regulation and control panel 501 is mainly controlled Dust removing units 200 and pulverizing unit 400 processed.
Further, in connection unit 100, the first external member 101 and the second external member 103 are respectively sleeved at two difference portions On part, locking piece 102 is reused afterwards to fix, the component connection played the role of;The pulverizer, which has, is provided with connection at three Unit 100, specifically, in the junction of pulverizing unit 400 and dust part 202, the connection of dust part 202 and collector unit 300 The junction of the air inducing part 201 of place and dust removing units 200 and dust part 202, makes stable connection at the connection outpost of the tax office, it is ensured that powder Broken machine can long-time service.
In dust removing units 200, dust removing units 200 are by 202 component of air inducing part 201 and dust part, specifically, such as Fig. 7 Shown, dust part 202 includes cylinder 103a and collection box 103b, and cylinder 103a is fixed on the top of collection box 103b, point Discharge pipe from cylinder 103a is connected with the blast pipe of air inducing part 201 by connection unit 100, specifically, the of connection unit 100 Sleeve piece 101 is set in the outside of the discharge pipe of cylinder 103a, and the second external member 103 of connection unit 100 is set in air inducing The outside of the blast pipe of part 201, afterwards the first external member 101 be fastened togather with the second external member 103, finally by locking piece 102 To rotate fixation;And air inducing part 201 is power part, the dust part 202 for dust removing units 200 collects dust, specifically , air inducing part 201 is suction ventilator, and when in use, air inducing part 201 powers on, it would be desirable to which the gas of dedusting is from collector unit 300 Inside it is adsorbed onto in dust part 202, dusty gas will form whirlwind in the cylinder 103a of dust part 202, utilize centrifugal force point From dust solid particle in air-flow, the dust solid particle separated is collected into collection box in the case where whirlwind rotation is sent In 103b, the dust in collection box 103b is focused on afterwards, make in this way dust removal efficiency can reach 97%, Using reliable, environmentally friendly, meet use demand.
In collector unit 300, including collection grain part 301 and separation member 302, collection grain part 301 are fixed on the bottom of separation member 302 End, both can be connected through a screw thread, specifically, separation member 302 plays methylbutanoic acid calcium particle centrifugation, and collect grain part 301 Playing the qualified particle diameter material of collection, separation member 302 distinguishes cylindrical drum and conically shaped again, and cylindrical drum is arranged on conically shaped top, and two Person is by solderable fixation, and the feed pipe of separation member 302 is connected with pulverizing unit 400, and the dust outlet tube of separation member 302 passes through company Order member 100 is connected with cylinder 103a into dirt pipe, and further, the first external member 101 of connection unit 100 is set in separation The dust outlet tube periphery of part 302, and the second external member 103 of connection unit 100 is set in the peripheral into dirt pipe of cylinder 103a, afterwards First external member 101 is fastened togather with the second external member 103, rotates fixation finally by locking piece 102, in use, in dedusting Under the action of the air inducing part 201 of unit 200, the methylbutanoic acid calcium crushed in pulverizing unit 400 will be drawn onto separation member 302 It is interior, air-flow containing grain will in separation member 302 interior formation whirlwind, utilize methylbutanoic acid calcium particle in centrifugal force separate air-flow, separation Methylbutanoic acid calcium particle out is collected into collection grain part 301 in the case where whirlwind rotation is sent, and separation rate can reach 97%, using reliable, Design is reasonable, meets use demand.
In pulverizing unit 400, including feed pieces 401 and driving part 402, feed pieces 401 play carrying and push away The effect of material is sent, and driving part 402 is the mechanism for crushing methylbutanoic acid calcium material, both cooperate, and effectively improve first The production efficiency of base calcium butyrate particle, specifically, feed pieces 401 include hopper, discharge port and pushing piece, before use, by first Base calcium butyrate material is placed in hopper, in use, the pushing piece of feed pieces 401 can lead to the methylbutanoic acid calcium material in hopper Cross discharge port to be pushed in driving part 402, pushing piece can be by electric pushrod and push plate component, and driving part 402 includes hitting Broken component 402a, adjusting part 402b and dispatch pipe 402c, as shown in figure 8, adjusting part 402b insertions are installed on and smash component In the discharge port of 402a, and dispatch pipe 402c spiral can be arranged on and smash on the outside of the discharge port of component 402a, in use, material from Smash component 402a feed inlet enter smash component 402a smash intracavitary, smash the driving motor of component 402a and will drive and hammer into shape Piece high-speed rotation, and then the effect of particle is smashed into material, effect of the material smashed in air inducing part 201 Under, the progress granule dust of separation member 302 that collector unit 300 is adsorbed onto by adjusting part 402b and dispatch pipe 402c is separated Process.
In control unit 500, including regulation and control panel 501 and cabinet 502, regulation and control panel 501 are arranged on cabinet 502, Therefore cabinet 502 plays the role of carrying, and regulate and control panel 501 and be mainly used for regulating and controlling the air inducing part 201 of dust removing units 200, crush The driving part 402 and air output of unit 400, regulation and control panel 501 include touch display screen, indicator light, starting switch.
The specific operation principle of the present embodiment is:Before use, power on, using connection unit 100 respectively by dedusting list Member 200 and collector unit 300, collector unit 300 and pulverizing unit 400 and the air inducing part 201 and dust of dust removing units 200 Part 202 is fixedly connected, then methylbutanoic acid calcium material is placed in the hopper of feed pieces 401, finally according to use demand, is made Air output is set with touch display screen, in use, opening the starting switch of regulation and control panel 501, the pushing piece of feed pieces 401 can Methylbutanoic acid calcium material in hopper is entered from the feed inlet for smashing component 402a smash component 402a smash intracavitary, smash The driving motor of component 402a will drive hammer leaf high-speed rotation, and then the effect of particle is smashed into material, smash Good material is adsorbed onto point of collector unit 300 by adjusting part 402b and dispatch pipe 402c under the action of air inducing part 201 Off member 302 carry out granule dust separation, air-flow containing grain will in separation member 302 interior formation whirlwind, utilize centrifugal force separate air-flow Middle methylbutanoic acid calcium particle, the methylbutanoic acid calcium particle separated is collected into collection grain part 301 in the case where whirlwind rotation is sent, due to gas Reason is flowed, dusty gas will be displaced into the cylinder 103a of dust part 202 from the dust outlet tube of separation member 302, and dusty gas will be Whirlwind is formed in the cylinder 103a of dust part 202, using dust solid particle in centrifugal force separate air-flow, is separated Dust solid particle whirlwind rotation send under, be collected into collection box 103b, afterwards in collection box 103b powder ash Dirt is focused on, and final clean gas is reached in air by the discharge of air inducing part 201.
Embodiment 5
It is in the present embodiment with previous embodiment difference:In order to realize the convenient dismounting and change of pipeline, behaviour is reduced The working strength of author, therefore in the junction of pulverizing unit 400 and dust part 202, the company of dust part 202 and collector unit 300 The air inducing part 201 of the place of connecing and dust removing units 200 is connected with the junction of dust part 202 using connection unit 100.
As shown in Fig. 9~13, in the present embodiment, connection unit 100 includes the first external member 101, locking piece 102 and second External member 103, specifically, the second external member 103 that the first external member 101 can be connected with it, wherein the first external member 101, second External member 103 may be contained within each segment pipe junction, and penetrating lock slots 101a is additionally provided with the first external member 101;Second set Part 103 includes the lock 103a and lock gear 103b for being located at 103 opposite flank of the second external member respectively, wherein lock 103a is " L " type is hook-shaped, and is inserted into lock slots 101a spin lockings, forms a screens groove between " L " type and the second external member 103 herein, when Second external member 103 along screens notch direction rotate when, lock 103a is slided in lock slots 101a, and screens groove is in lock slots Gap in 101a gradually decreases, the two final inconsistent lock realized between the first external member 101 and the second external member 103 in bottom It is fixed, preferably, being also provided with guide surface on lock 103a, lock 103a is entered in lock slots 101a and is play the guiding role;
In order to which the second external member 103 is fixedly connected on pipeline, so that by rotating the second external member 103, with the first external member 101 fix, and realize the connection between pipeline.The pipe end 600 being connected with the second external member 103 includes docking extended loop 601, ring Groove 602 and limiting slot 603, specifically, docking extended loop 601 is docked with the first external member 101, annular groove 602 is arranged at docking extension On the interface of ring 601, and the second external member 103 is arranged in annular groove 602, and limiting slot 603 is arranged at the side opposite with interface On face, and lock gear 103b is located in limiting slot 603, in the present embodiment for the second external member 103 and the pipe being directly connected to Fixation between road, wherein be additionally provided with screw 103c in the second external member 103, the second external member 103 is with docking between extended loop 601 Connected by screw 103c, and screw 103c is located in limiting slot 603 and slides spacing, further, screw 103c includes screw Head and screw bar portion, and the internal diameter of screw bar portion is matched with the groove internal diameter of lock slots 101a, and the length of screw bar portion but with The groove depth of lock slots 101a matches, and is fixed so that screw bar portion passes through in lock slots 101a with the second external member 103, works as rotation During the second external member 103, screw bar portion can move in lock slots 101a, and spacing by screw head;Therefore preferable screw 103c is hex screw, for by the spacing fixation between the first external member 101 and the second external member 103;
In order to by the second external member of rotation 103 of device simple and fast, reduce the labor intensity of operator, connection unit 100 further include locking piece 102, specifically, locking piece 102 is is arranged on pipeline, it further includes rotation gear 102a, turntable 102b and supporting block 102c, rotates gear 102a and lock gear 103b and coordinates the rotation for driving the second external member 103, certainly originally It can also be that further, turntable 102b passes through shaft along the rotating swingle of central point that rotating mode is realized in embodiment It is connected with rotation gear 102a, supporting block 102c is arranged on docking extended loop 601, and is in same side with limiting slot 603 On, fixed between rotation gear 102a and turntable 102b by supporting block 102c, rotating process is in the present embodiment:Operator Turntable 102b is rotated manually and drives the rotation of rotation gear 102a, and is rotated gear between gear 102a and lock gear 103b and connected It is dynamic, so as to drive the rotation of the second external member 103, enter spacing completion in lock slots 101a when rotating rear catch 103a to a certain degree The process of locking, and the process dismantled need to only rotate backward turntable 102b, the process simple and fast, will produce during installing and dismounting Raw longitudinal force is converted into rotation torque power, not only installing and dismounting simple and fast, while the also significantly relatively low work of operator Intensity
Embodiment 6
It is in the present embodiment with previous embodiment difference:The outlet of driving part 402 is provided with adjusting part 402b, By adjusting part 402b due to being changed be subject to wind-force size so as to automatically adjust the size that driving part 402 exports, so that Wind-force in pipeline is maintained to stable given state, ensure that the stability of crushing material particle diameter.
As shown in Figure 14~17, in the present embodiment, adjusting part 402b matches somebody with somebody including the first counterpart 402b-10, second Component 402b-20, rebound part 402b-30 and fixing piece 402b-40.First counterpart 402b-10 and the second counterpart 402b- 20 interspersed connections, the first counterpart 402b-10 are arranged on fixing piece 402b-40 by springing back part 402b-30, and second coordinates Part 402b-20 and fixing piece 402b-40 is interconnected.
Specifically, the first counterpart 402b-10 plays the role of promoting the second counterpart 402b-20 to carry out eccentric rotary. First counterpart 402b-10, which includes circle magnetic patch 402b-11 and interlocking bar 402b-12, circular magnetic patch 402b-11, has magnetism, Planform is circle, and centre position has a circular hole.Interlocking bar 402b-12 has four, and interlocking bar 402b-12 is wherein One end is fixed on circular magnetic patch 402b-11, and other end is outward-dipping in a corresponding plane, and the plane is by linkage On the straight line that contact points of the bar 402b-12 on circular magnetic patch 402b-11 is linked to be with the center of circle, and the plane is perpendicular to circular magnetic Plane where block 402b-11.Four interlocking bar 402b-12 are evenly distributed on the surface of circular magnetic patch 402b-11, preferably, The angle of inclination of four interlocking bar 402b-12 is identical, is centrosymmetric mutually, and four contact points are also distributed in diameter one at the same time On fixed circumference.
Second counterpart 402b-20 has the air inlet for covering dispatch pipe 402c, determines the effect of gas flow size.The Two counterpart 402b-20 are circular contour, similarly have four, and four shape and structure phases corresponding to interlocking bar 402b-12 Together.It is connected by the way that shaft 402b-21 and fixing piece 402b-40 are eccentric, and eccentric rotation can be carried out around shaft 402b-21 Turn.Second counterpart 402b-20 has hole 402b-22, four interlocking bar on the opposite side of diameter where shaft 402b-21 Correspondence is extend into four hole 402b-22 of the second counterpart 402b-20 respectively for the outer end of 402b-12, forms linkage.
Rebound part 402b-30 has carries out rebound playback by the first counterpart 402b-10 and the second counterpart 402b-20 Effect.Springing back part 402b-30 includes telescopic shaft 402b-31, base 402b-32, compression spring 402b-33 and spring leaf 402b-34.One end of telescopic shaft 402b-31 is connected with base 402b-32, and fixed, and the other end is provided with a port, holds Mouth is circle, and diameter is more than the outside diameter of telescopic shaft 402b-31.Compression spring 402b-33 is sheathed on telescopic shaft 402b-31, and two End is limited by the port of base 402b-32 and telescopic shaft 402b-31;Spring leaf 402b-34 corresponds to four second cooperations Part 402b-20 has four, and shape is identical, is " V " shape spring leaf.One side of spring leaf 402b-34 is longer, while compared with Short, shorter one end is fixed on the edge of base 402b-32, and longer one end deviates from base 402b-32, towards outside, and supports In the outer edge of corresponding second counterpart 402b-20.In structure, the spring leaf 402b-34 after fixing is in inverted " v ".Need It is noted that on the circular magnetic patch 402b-11 of the first counterpart 402b-10, Circularhole diameter is slightly larger than telescopic shaft 402b-31 Outer diameter.Meanwhile circular magnetic patch 402b-11 is sheathed on telescopic shaft 402b-31 by circular hole thereon, is simultaneously propped up and is stretched The port of contracting axis 402b-31, another side prop up compression spring 402b-33.
Fixing piece 402b-40 has the function that fixed whole adjusting part 402b, its outer contour is circle, at two mutually Vertical diametrically has connecting rod, and two connecting rods are vertically compared to the center of circle, and circle centre position has certain space to put Put and fix the base 402b-32 of rebound part 402b-30.Space between connecting rod is used for the circulation of gas.
In the present embodiment, adjusting part 402b can control the first counterpart 402b-10 by the effect of external magnetic field Movement so that the size for the mechanisms influence air flow rate for passing through linkage.Detailed process includes the following steps:
First, external magnetic field (magnetic flexible) strengthens, and the circular magnetic patch 402b-11 being sheathed on telescopic shaft 402b-31 is subject to magnetic The repulsive force effect of power circle is moved inward along telescopic shaft 402b-31.
2nd, the magnetic flexible of movement drives the interlocking bar 402b-12 being fixed thereon to be moved at the same time, due to interlocking bar The other end of 402b-12 is interspersed in the hole 402b-22 of the second counterpart 402b-20, therefore drives the second counterpart 402b- 20 eccentric rotaries of 402b-21 progress around the shaft, the direction of rotation is the inner side of device.
3rd, the second counterpart 402b-20 of eccentric rotary gradually blocks the inlet air of a part of dispatch pipe 402c inwardly The area of mouth, so as to have impact on the size of gas flow.
4th, continue to increase magnetic field, until repulsive force caused by external magnetic field is equal to the bounce of spring leaf 402b-34 or waits In the sum of holding power that the bounce and base 402b-32 of spring leaf 402b-34 provide, the flow of gas is minimum at this time.
5th, magnetic field is reduced, repulsive force caused by magnetic field is relatively reduced, and the first counterpart 402b-10 is subject to compress spring The bounce of 402b-33 moves out, at the same the second counterpart 402b-20 be subject to the effects of spring leaf 402b-34 bounces to Outer eccentric rotary, whole device gradually playback.
6th, during device playback, the area that the second counterpart 402b-20 covers the air inlet of dispatch pipe 402c subtracts Few, gas flow becomes larger.
It should be understood that this application is not limited to details or method being illustrated in the description of the above or being illustrated in figure.Also It should be understood that wording and term are only in order at description purpose and are not considered as limitation used by herein.
It is important that, it should be noted that the construction and arrangement of the application shown in multiple and different exemplaries is only It is illustrative.Although several embodiments are only described in detail in this disclosure, the personnel of the displosure content are referred to It should be easily understood that on the premise of substantially without departing from the novel teachings and advantage of the theme described in this application, many changes Type is possible (for example, the size of various parts, scale, structure, shape and ratio and parameter value are (for example, temperature, pressure Deng), mounting arrangements, the use of material, the change etc. of color, orientation).Can be by more for example, being shown as integrally formed element A part or element are formed, and the position of element can be squeezed or change in other ways, and the property or number of discrete component Or position can be altered or changed.Therefore, all such remodeling are intended to be comprised in the scope of the present invention.Can according to for The embodiment in generation changes or the order or order of resequence any process or method and step.In the claims, any " dress Put plus function " clause be intended to be covered in it is described herein perform the structure of the function, and be not only structure and be equal But also it is equivalent structure.Without departing from the scope of the invention, design, operation that can be in exemplary Other are made in situation and arrangement to replace, retrofit, change and omit.Therefore, the present invention is not restricted to specific embodiment, and It is to extend to a variety of remodeling still fallen within the scope of the appended claims.
In addition, in order to provide the terse description of exemplary, all spies of actual implementation scheme can not be described Sign (that is, with currently consider execution the present invention those incoherent features of optimal mode, or in realize the present invention it is incoherent Those features).It should be understood that in the development process of any actual implementation mode, such as in any engineering or design object, Substantial amounts of embodiment can be made to determine.Such development effort is probably complicated and time-consuming, but is obtained for those For the those of ordinary skill of the displosure content, it is not necessary to which excessive experiment, the development effort will be a design, manufacture With the routine work of production.
It should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to preferable The present invention is described in detail in embodiment, it will be understood by those of ordinary skill in the art that, can be to the technology of the present invention Scheme technical scheme is modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention, it should all cover in this hair Among bright right.

Claims (10)

  1. A kind of 1. preparation method of beta-hydroxy-Beta-methyl calcium butyrate, it is characterised in that:Including,
    Sulfuric acid, glacial acetic acid, hydrogen peroxide are mixed, Peracetic acid is collected in an isothermal reaction, distillation;
    The Peracetic acid is mixed with diacetone alcohol, addition methyl acetate, secondary isothermal reaction, distillation collection beta-hydroxy-β- Methylbutanoic acid;
    Add water to the beta-hydroxy-Beta-methyl butyric acid, after adjusting pH value of solution, dissolve by heating filtering, take filtrate to add calcium chloride, stir Reaction is mixed, adjusts pH, separates out beta-hydroxy-Beta-methyl calcium butyrate, is filtered, drying, obtains beta-hydroxy-Beta-methyl calcium butyrate, carries out Ultramicro grinding obtains product.
  2. 2. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:Constant temperature Reaction, its be temperature be 40~50 DEG C, mixing speed be 200~250rpm, reaction 8~12min.
  3. 3. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The secondary constant temperature Reaction, its be temperature be 25~35 DEG C, mixing speed be 80~120rpm, reaction 50~70min.
  4. 4. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The stirring reaction, It is 20~30min of stirring reaction under 350~450rpm.
  5. 5. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The adjusting solution PH, its be by solution adjust to pH be 5.8~6.2.
  6. 6. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The adjusting pH, its It is that pH is adjusted most 6.3~6.7.
  7. 7. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The sulfuric acid quality Concentration is 8~15%, and the volume ratio of itself and glacial acetic acid is 1:8~10.
  8. 8. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The hydrogen peroxide Mass concentration is 25~35%, and the volume ratio of itself and glacial acetic acid is 2.5~3.5:1.
  9. 9. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The distillation is collected Peracetic acid, it is that the cut of 60 DEG C of vacuum distillation collection obtains Peracetic acid.
  10. 10. the preparation method of beta-hydroxy-Beta-methyl calcium butyrate according to claim 1, it is characterised in that:The distillation is collected Beta-hydroxy-Beta-methyl butyric acid, it is that 70 DEG C of cut is collected in distillation, obtains methyl acetate, the material after distillation for beta-hydroxy-β- Methylbutanoic acid solution.
CN201711166893.7A 2017-11-21 2017-11-21 A kind of preparation method of beta-hydroxy-Beta-methyl calcium butyrate Withdrawn CN107954855A (en)

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Publication number Priority date Publication date Assignee Title
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