CN100999459B - Technology of synthesizing nano bismuth stearate by liquid phase dispersing process - Google Patents
Technology of synthesizing nano bismuth stearate by liquid phase dispersing process Download PDFInfo
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- CN100999459B CN100999459B CN2007100342507A CN200710034250A CN100999459B CN 100999459 B CN100999459 B CN 100999459B CN 2007100342507 A CN2007100342507 A CN 2007100342507A CN 200710034250 A CN200710034250 A CN 200710034250A CN 100999459 B CN100999459 B CN 100999459B
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Abstract
This invention relates to a technology of using liquid-phase dispersion method to synthesize nanometer stearate Bismuth, belongs to stearic acid metal salts field. Its process: first will add the reactor of stearic acid, atmospheric heating to melt; second will add dispersant of the same amount as stearic acid to reactor, mixing them; the third step is under continuously mixing conditions, slowly add bismuth carbonate of 1.01 to 1.02 times of theory demand amount, and maintain a constant temperature, to synthesize stearic acid bismuth suspended emulsion; forth will centrifugal separate the stearic acid bismuth suspended emulsion, drying to gain micron stearate bismuth; at last send micro-stearate Bismuth to smash equipment, through airflow, finally obtain nanometer-stearate bismuth products. This invention has good dispersion, and high purity, big coverage, access to gastrointestinal lesions. It can diffuse directly to form protective layer, promoting mucosa and mucosal ulcer healing, is a brand new structure of the mucosal protective agent, can be a category of new drugs.
Description
Technical field
The present invention relates to the bismuth preparation production technique, belong to the Metallic stearates field, the technology of a kind of synthesizing nano bismuth stearate by liquid phase dispersing process of more specifically saying so.
Background technology
It has often been said " people eats five cereals, and who can not have disease ", and the diet inlet, at first influence is exactly stomach.And along with the development of society, people's survival pressure is increasing, and because of reasons such as work, lives, gastrointestinal disorder patient's ratio is in continuous increase, and according to incompletely statistics, global gastrointestinal disorder patient accounts for more than 10% of total number of persons.As the saying goes the living all kinds of diseases and ailments of stomach trouble, therefore,, the treatment of gastrointestinal disorder has been caused more experts and scholars' research in the face of vast gastrointestinal disorder patient colony like this.It is peptide ulceration (stomach ulcer and duodenal ulcer) that suitable major part is arranged among the gastrointestinal disorder patient; mucosa protective agent based on bismuth preparation is one of main medicine of present peptic gastric ulcer, mainly contains Bisuc, bismuth pectin, Vikaline, colloidal bismuth subcitrate, bismuth citrate and Bismuth Potassium Citrate etc.These organic acid bismuth salt are behind quantitative hot water dissolving; form the solution shape after the gastric juice hydrolysis; utilize organic acid bismuth salt in biology table body, to have effect slow, controlled release; generate the very small effective ingredient precipitation of granularity; the protective layer that forms dispersivity is covered on the ulcer surface; protection protection stomach mucous membrane, ulcer surface promote ulcer mucosa regeneration and ulcer healing.The granularity of its effective ingredient is more little, quality is light more, it is dispersed just good more, the easy more protective layer that enters gastroenteritic ulcer place formation dispersivity.Stearic acid is the monovalence organic acid; stearic acid and monovalence BiO are combined to nano bismuth stearate; nano bismuth stearate molecule granularity is little; light weight; good dispersity; in biology table body, have be better than above-mentioned bismuth preparation delay release, absorption, dispersion and metabolism performance, enter the protective layer that the gastroenteritic ulcer place can be formed directly in dispersivity, reduce in addition gastric content acidity, in and the effect of hydrochloric acid in gastric juice.But do not see the synthetic method report of relevant nano bismuth stearate so far.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of technology of synthesizing nano bismuth stearate by liquid phase dispersing process, to develop deeper organic acid bismuth industry.
In order to address the above problem, of the present inventionly be contemplated that substantially:
Under agitation, Bismuth Subcarbonate is dispersed into smaller particles in stearic acid fusing, and its BiO is owing to have higher internal cohesive energy and bigger surface tension; Therefore less BiO surface has very high reactive behavior, and is reflected at the protective layer that less particle surface forms stearate with stearic acid; In case particle surface splits, had the spatial obstacle layer around the stearate, the gathering between BiO just can be prevented effectively; These protected smaller particles can little by little be dispersed into littler particle, and final formation is similar to the emulsion mixed system; This emulsion drying, comminution by gas stream just can obtain the nano bismuth stearate particulate.
Chemical equation is as follows:
(BiO)
2CO
3·1/2H
2O+2C
17H
35COOH→2(BiO)(C
17H
35COO)+CO
2↑+1
1/
2H
2O↑
BiO (C wherein
17H
35COO) be bismuth stearate, molecular weight 508.5, bismuth-containing 41.10%, bismuth oxide-containing 44.25% contains stearic acid 55.75%, and purity is more than 99.5%.White superfine powder, granularity to the micron again to nano level.
Technical scheme to be solved by this invention is: a kind of technology of synthesizing nano bismuth stearate by liquid phase dispersing process is to carry out as follows:
(1) stearic acid is added in the reactor, the normal pressure heat temperature raising is to fusing;
(2) get 0.5～1% the dispersion agent that adds weight by stearic acid and mix in the reactor, mix and stir;
(3) under continuous stirring condition, slowly add the Bismuth Subcarbonate of 1.01～1.02 times of theoretical requirements, when heating to 100～102 ℃, constant temperature, synthetic bismuth stearate suspended emulsion;
(4) with the centrifugation of synthetic bismuth stearate suspended emulsion, oven dry obtains the micron order bismuth stearate;
(5) the micron order bismuth stearate is sent in the disintegrating apparatus,, finally obtained the nano bismuth stearate product through comminution by gas stream.
Repeatedly test through the contriver, four principal elements that influence the present invention's realization are:
(1) reaction times
The length in reaction times is directly connected to the height whether reaction reaches product purity fully.Reaction times should be not more than 90min, and the reaction times, less than the 30min reaction not exclusively it was meaningless to reacting itself to surpass 90min, can make the production cycle elongated on the contrary, and product colour is deepened.
(2) temperature of reaction
This temperature of reaction can be carried out in wide temperature range, but that reaction temperature is spent is low, often makes reaction not exclusively, cause the product free acid to increase, the raising temperature helps reaction carries out fully, but the too high meeting of temperature is deepened product colour, and both all influence quality product.
Analytical results shows that when temperature of reaction was lower than 100 ℃, free acid content increased the quality instability in the product; Product colour deepens when being higher than 105 ℃.
(3) dispersion agent class and dispersant dosage
Glycerol, Virahol, anhydrous sorbitol etc. and mixture all can be made dispersion agent.Dispersant dosage has a significant impact reaction, and best dispersion effect is arranged in how many scopes of consumption, is that one of problem of exploring meaning is arranged most.Dispersant dosage is selected 0.5～1% of stearic acid add-on for use.
(4) terminal point of reaction control
Even synthetic by above-mentioned optimum process condition, entire reaction course still needs strict control.Reaction conditions is changed.The terminal point control of this reaction is most important, the acid number control of the analysed preparation of can taking a sample in the production.
The present invention has following beneficial effect:
The finished product-nano bismuth stearate of the present invention; has clear superiority with traditional its chemical stability of bismuth preparation comparison and powder size; stearic acid of the present invention and monovalence BiO are combined to nano bismuth stearate; the molecule granularity is little; to nano level; do not need to dissolve again; light weight, good dispersity, purity height; wide coverage; enter the stomach and intestine lesion, directly form the dispersivity protective layer, promote mucous membrane to tie again and ulcer healing; be a kind of mucosa protective agent of brand new, can be used as the first class national new drug exploitation.
The present invention is not reaction medium with water with the synthetic bismuth stearate of liquid phase dispersion method, do not add the sodium salt that influences quality product yet, so product need not washing, production process does not have waste water and produces, advantage such as have that technical process is simple, facility compact, simple to operate, constant product quality, production cost are low.
Description of drawings
Describe the present invention below in conjunction with accompanying drawing in detail with specific embodiment:
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
A kind of technology of synthesizing nano bismuth stearate by liquid phase dispersing process, its technical process is carried out as follows:
(1) stearic acid is added in the reactor 70～88 ℃ of extremely fusings of normal pressure heat temperature raising;
(2) 1% the dispersion agent-edible glycerol of getting by the stearic acid add-on is mixed in the reactor, is mixed and stirred 15 minutes;
(3) under continuous stirring condition, slowly add Bismuth Subcarbonate through metering, when heating to 100～102 ℃, constant temperature, controlling reaction time 40～70 minutes, synthetic bismuth stearate suspended emulsion;
Wherein the add-on of Bismuth Subcarbonate is controlled at 1.01～1.02 times of theoretical requirement and is advisable, in the unit weight stearic acid and the weight G that adds alkali formula bismuth stearate be calculated as follows:
G＝[H×M×(1.01～1.02)]/56.1×100×2×X
In the formula: the stearic acid number of H-, mgKOH/g;
The content of X-Bismuth Subcarbonate;
M-Bismuth Subcarbonate (BiO)
2CO
3.1/2H
2The molecular weight of O;
56.1-the molecular weight of potassium hydroxide KOH;
(4) with the centrifugation of synthetic bismuth stearate suspended emulsion, arrange liquid of the residual end, get the upper strata emulsion and obtain the micron order bismuth stearate through 90～100 ℃ of oven dry;
(5) the micron order bismuth stearate is sent in the disintegrating apparatus,, finally obtained the nano bismuth stearate product through comminution by gas stream.
Embodiment 2
A kind of technology of synthesizing nano bismuth stearate by liquid phase dispersing process is characterized in that: technical process is carried out as follows:
(1) stearic acid is added in the reactor 75～85 ℃ of extremely fusings of normal pressure heat temperature raising;
(2) 0.5% the Virahol of getting by the stearic acid add-on mixes in the reactor, mixes and stirs 10 minutes;
(3) under continuous stirring condition, slowly add Bismuth Subcarbonate through metering, when heating to 100～102 ℃, constant temperature, controlling reaction time 55～75 minutes, synthetic bismuth stearate suspended emulsion;
Wherein the add-on of Bismuth Subcarbonate is controlled at 1.01～1.02 times of theoretical requirement and is advisable, in the unit weight stearic acid and the weight G that adds alkali formula bismuth stearate be calculated as follows:
G＝[H×M×(1.01～1.02)]/56.1×100×2×X
In the formula: the stearic acid number of H-, mgKOH/g;
The content of X-Bismuth Subcarbonate;
M-Bismuth Subcarbonate (BiO)
2CO
3.1/2H
2The molecular weight of O;
56.1-the molecular weight of potassium hydroxide KOH;
(4) with the centrifugation of synthetic bismuth stearate suspended emulsion, arrange liquid of the residual end, get the upper strata emulsion and obtain the micron order bismuth stearate through 95～105 ℃ of oven dry;
(5) the micron order bismuth stearate is sent in the disintegrating apparatus,, finally obtained the nano bismuth stearate product through comminution by gas stream.
Embodiment 3
A kind of technology of synthesizing nano bismuth stearate by liquid phase dispersing process is characterized in that: technical process is carried out as follows:
(1) stearic acid is added in the reactor 85～90 ℃ of extremely fusings of normal pressure heat temperature raising;
(2) 0.8% the anhydrous sorbitol of getting by the stearic acid add-on mixes in the reactor, mixes and stirs 20 minutes;
(3) under continuous stirring condition, slowly add Bismuth Subcarbonate through metering, when heating to 100～102 ℃, constant temperature, controlling reaction time 60～80 minutes, synthetic bismuth stearate suspended emulsion;
Wherein the add-on of Bismuth Subcarbonate is controlled at 1.01～1.02 times of theoretical requirement and is advisable, in the unit weight stearic acid and the weight G that adds alkali formula bismuth stearate be calculated as follows:
G＝[H×M×(1.01～1.02)]/56.1×100×2×X
In the formula: the stearic acid number of H-, mgKOH/g;
The content of X-Bismuth Subcarbonate;
M-Bismuth Subcarbonate (BiO)
2CO
3.1/2H
2The molecular weight of O;
56.1-the molecular weight of potassium hydroxide KOH;
(4) with the centrifugation of synthetic bismuth stearate suspended emulsion, arrange liquid of the residual end, get the upper strata emulsion and obtain the micron order bismuth stearate through 100～110 ℃ of oven dry;
(5) the micron order bismuth stearate is sent in the disintegrating apparatus,, finally obtained the nano bismuth stearate product through comminution by gas stream.
Claims (4)
1. the technology of a synthesizing nano bismuth stearate by liquid phase dispersing process, it is characterized in that: technical process is carried out as follows:
(1) stearic acid is added in the reactor, the normal pressure heat temperature raising is to fusing;
(2) get 0.5～1% the dispersion agent that adds weight by stearic acid and mix in the reactor, mix and stir;
(3) under continuous stirring condition, slowly add the Bismuth Subcarbonate of 1.01～1.02 times of theoretical requirements, when heating to 100～102 ℃, constant temperature, synthetic bismuth stearate suspended emulsion;
(4) with the centrifugation of synthetic bismuth stearate suspended emulsion, oven dry obtains the micron order bismuth stearate;
(5) the micron order bismuth stearate is sent in the disintegrating apparatus,, finally obtained the nano bismuth stearate product through comminution by gas stream.
2. the technology of synthesizing nano bismuth stearate by liquid phase dispersing process according to claim 1 is characterized in that: the dispersion agent in described (2) step is edible glycerol.
3. the technology of synthesizing nano bismuth stearate by liquid phase dispersing process according to claim 1, it is characterized in that: the dispersion agent in described (2) step is a Virahol.
4. the technology of synthesizing nano bismuth stearate by liquid phase dispersing process according to claim 1, it is characterized in that: the dispersion agent in described (2) step is an anhydrous sorbitol.
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| CN2007100342507A CN100999459B (en) | 2007-01-12 | 2007-01-12 | Technology of synthesizing nano bismuth stearate by liquid phase dispersing process |
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| CN100999459B true CN100999459B (en) | 2010-12-01 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793101A (en) * | 2005-12-23 | 2006-06-28 | 华东师范大学 | Process for hydrothermal synthesizing bismuth citrate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793101A (en) * | 2005-12-23 | 2006-06-28 | 华东师范大学 | Process for hydrothermal synthesizing bismuth citrate |
Non-Patent Citations (2)
| Title |
|---|
| JP平5-331096A 1993.12.14 |
| 赵彦保等.液相分散法制备硬脂酸修饰铋纳米微粒.《无机化学学报》.2003,第19期(第9期),997-1000. * |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20070803 Address after: Hunan Province, Chenzhou City Road, No. 1 gold Applicant after: Jinwang Industry Co., Ltd., Hunan Address before: Hunan Province, Chenzhou City Road, No. 1 gold Applicant before: Jinwang Industrial Co., Ltd., Chenzhou |
|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: HU'NAN JINWANG BISMUTH INDUSTRY PLC Free format text: FORMER OWNER: JINWANG INDUSTRY CO., LTD., HUNAN Effective date: 20111207 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20111207 Address after: 423000 Chenzhou City, Hunan province Bailu town export processing zone Jinwang company Patentee after: Hunan Jinwang Bismuth Co.,Ltd. Address before: 423000 Hunan Province, Chenzhou City Road, No. 1 gold Patentee before: Jinwang Industry Co., Ltd., Hunan |
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| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101201 Termination date: 20110112 |
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| C49 | Reinstatement of patent right or utility model | ||
| RR01 | Reinstatement of patent right |
Former decision: cessation of patent right due to non-payment of the annual fee Former decision publication date: 20120328 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101201 Termination date: 20180112 |
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| CF01 | Termination of patent right due to non-payment of annual fee |