CN109734109A - A method of preparing ethoxy-dithioformic acid Intercalated - Google Patents
A method of preparing ethoxy-dithioformic acid Intercalated Download PDFInfo
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- CN109734109A CN109734109A CN201910158609.4A CN201910158609A CN109734109A CN 109734109 A CN109734109 A CN 109734109A CN 201910158609 A CN201910158609 A CN 201910158609A CN 109734109 A CN109734109 A CN 109734109A
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- acid intercalated
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Abstract
The invention discloses a kind of methods for preparing ethoxy-dithioformic acid Intercalated, comprising the following steps: A, carries out weighing dissolution according to the ratio of molar ratio 2: 1 by Aluminium chloride hexahydrate and Magnesium dichloride hexahydrate, obtains mixed solution A；B, urea and sodium ethylxanthate are carried out weighing dissolution according to the ratio of molar ratio 4: 1, obtains mixed solution B；C, mixed solution B is placed in reaction vessel, mixed solution A is gradually added dropwise in mixed solution B, mixed solution B is stirred at the same time, when mixed solution A is added dropwise to the 50% of its total amount, sodium hydroxide solution is added dropwise into mixed solution B while mixed solution A is added dropwise；D, accelerate mixing speed after being added dropwise, persistently stir 2h, be then allowed to stand 12h；E, the solution after standing filtered, dried, ground, obtain pale yellow powder shape hydrotalcite.The present invention can improve the deficiencies in the prior art, improve the crystal structure of ethoxy-dithioformic acid Intercalated.
Description
Technical field
The present invention relates to hydrotalcite technical field, especially a kind of side for preparing ethoxy-dithioformic acid Intercalated
Method.
Background technique
Hydrotalcite is a kind of inorganic material with anion stratiform function, has variable chemical composition and performance, quilt
It is widely used in the insulation of various types of materials, in the multiple fields such as fire-retardant, anti-aging.Magnalium hydrotalcite is a kind of common neatly
Stone.Ethoxy-dithioformic acid Intercalated is a kind of magnalium hydrotalcite of modification, can provide the anti-oxidant of magnalium hydrotalcite
Protection effect.Ethoxy-dithioformic acid Intercalated generallys use traditional double drop coprecipitations and is prepared.But pass through
The ethoxy-dithioformic acid Intercalated crystal structure that this method prepares is more loose, causes its protection effect cannot
It is satisfactory.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method for preparing ethoxy-dithioformic acid Intercalated, energy
The deficiencies in the prior art are enough solved, the crystal structure of ethoxy-dithioformic acid Intercalated is improved.
In order to solve the above technical problems, the technical solution used in the present invention is as follows.
A method of preparing ethoxy-dithioformic acid Intercalated, comprising the following steps:
A, Aluminium chloride hexahydrate and Magnesium dichloride hexahydrate are weighed according to the ratio of molar ratio 2: 1, is then added and goes
It is dissolved in ionized water, obtains mixed solution A；
B, urea and sodium ethylxanthate are weighed according to the ratio of molar ratio 4: 1, is then added in deionized water
It is dissolved, obtains mixed solution B；
C, mixed solution B is placed in reaction vessel, mixed solution A is gradually added dropwise in mixed solution B, it is same with this
When mixed solution B is stirred, 25 DEG C when the temperature in reaction vessel is by being added dropwise are linearly increasing to completion of dropwise addition and are
75 DEG C, when mixed solution A is added dropwise to the 50% of its total amount, be added dropwise while mixed solution A is added dropwise into mixed solution B
Sodium hydroxide solution, the dropwise addition of sodium hydroxide solution and the dropwise addition of mixed solution A terminate simultaneously, the sodium hydroxide of dropwise addition and dropwise addition
Urea molar ratio be 1: 10；
D, accelerate mixing speed after being added dropwise, persistently stir 2h, be then allowed to stand 12h；
E, the solution after standing is filtered, and filter cake is washed with deionized to neutrality, the dry 12h at 80 DEG C,
Filter cake is taken out, grinding obtains pale yellow powder shape hydrotalcite, as ethoxy-dithioformic acid Intercalated.
Preferably, the molar ratio of aluminium chloride and deionized water is 2: 25 in mixed solution A, and in mixed solution B, ethyl
The molar ratio of sodium xanthogenate and deionized water is 1: 40.
Preferably, in step C, mixing speed 120rad/min；In step D, mixing speed 350rad/min.
Preferably, in step D, solution temperature when standing is maintained at 40 DEG C.
It is protected preferably, being filled with nitrogen in step C and step D, in reaction vessel.
Preferably, the reaction vessel includes cavity, the bottom of cavity is provided with inclined-plane, and the left-hand end on inclined-plane is higher than the right side
Side is equipped with drop tube above inclined-plane left-hand end, and the end of drop tube is connected with several dropwise addition heads arranged side by side, tiltedly
Right side of face is equipped with agitating paddle above end.
Preferably, the side wall of the drop tube is equipped with primary heater, secondary heater is installed in inclined-plane.
Brought beneficial effect is by adopting the above technical scheme: the present invention is carried out using the method that urea decomposes precipitating
The preparation of ethoxy-dithioformic acid Intercalated.On this basis, yellow using excess urea and ethyl by the phase before the reaction
Ortho acid sodium solution, the phase adds highly basic and changes reaction temperature after the reaction, the resolution ratio of urea is gradually increased, to improve crystallization
Degree improves crystal structure.At crystalline deposit initial stage, mixing slowly can make nucleus more uniform；In the crystalline deposit later period, quickly
Stirring can accelerate crystallization rate, improve the global consistency of crystal grain.In order to further increase the uniformity of crystallization reaction, this hair
Bright specially to devise a kind of reaction vessel, bottom is inclined-plane, carries out the dropwise addition of mixed solution in the higher one end in position, utilizes
Difference in height realizes the quick mixing between solution, and then in the lower one end in position, (main region of crystallization reaction) is stirred
It mixes, whipping process can be improved for the mixing effect in crystallization reaction region.
Detailed description of the invention
Fig. 1 is the ethoxy-dithioformic acid Intercalated that a specific embodiment and comparative example of the invention prepare
XRD spectrum.
Fig. 2 is the SEM figure for the ethoxy-dithioformic acid Intercalated that a specific embodiment of the invention prepares.
Fig. 3 is the SEM figure for the ethoxy-dithioformic acid Intercalated that comparative example prepares.
Fig. 4 is the structure chart of reaction vessel in a specific embodiment of the invention.
Fig. 5 is the structure chart that head is added dropwise in a specific embodiment of the invention.
Specific embodiment
The specific embodiment of the present invention the following steps are included:
A, Aluminium chloride hexahydrate and Magnesium dichloride hexahydrate are weighed according to the ratio of molar ratio 2: 1, is then added and goes
It is dissolved in ionized water, obtains mixed solution A；
B, urea and sodium ethylxanthate are weighed according to the ratio of molar ratio 4: 1, is then added in deionized water
It is dissolved, obtains mixed solution B；
C, mixed solution B is placed in reaction vessel, mixed solution A is gradually added dropwise in mixed solution B, it is same with this
When mixed solution B is stirred, 25 DEG C when the temperature in reaction vessel is by being added dropwise are linearly increasing to completion of dropwise addition and are
75 DEG C, when mixed solution A is added dropwise to the 50% of its total amount, be added dropwise while mixed solution A is added dropwise into mixed solution B
Sodium hydroxide solution, the dropwise addition of sodium hydroxide solution and the dropwise addition of mixed solution A terminate simultaneously, the sodium hydroxide of dropwise addition and dropwise addition
Urea molar ratio be 1: 10；
D, accelerate mixing speed after being added dropwise, persistently stir 2h, be then allowed to stand 12h；
E, the solution after standing is filtered, and filter cake is washed with deionized to neutrality, the dry 12h at 80 DEG C,
Filter cake is taken out, grinding obtains pale yellow powder shape hydrotalcite, as ethoxy-dithioformic acid Intercalated.
In mixed solution A, the molar ratio of aluminium chloride and deionized water is 2: 25, in mixed solution B, sodium ethylxanthate with
The molar ratio of deionized water is 1: 40.
In step C, mixing speed 120rad/min；In step D, mixing speed 350rad/min.
In step D, solution temperature when standing is maintained at 40 DEG C.
Nitrogen is filled in step C and step D, in reaction vessel to be protected.
Referring to Fig. 4-5, reaction vessel includes cavity 1, and the bottom of cavity 1 is provided with inclined-plane 2, and the left-hand end on inclined-plane 2 is higher than
Right-hand end is equipped with drop tube 3 above 2 left-hand end of inclined-plane, and the end of drop tube 3 is connected with several dropwise additions arranged side by side
First 4, agitating paddle 7 is installed above 2 right-hand end of inclined-plane.The side wall of drop tube 3 is equipped with primary heater 8, installation in inclined-plane 2
There is secondary heater 9.
It is provided with necking part 5 in addition, being added dropwise in head 4, the bottom edge that head 4 is added dropwise is provided with toothed region 6.The structure that head is added dropwise can
To increase the diameter of dropwise addition process drop, to improve the mixing velocity after liquid is fallen in mixed solution.
Comparative example (double drop coprecipitations)
(1) it is 3: 1 by Mg/Al molar ratio, weighs a certain amount of magnesium salts and aluminium salt, it is completely molten that 100ml deionized water is added
Solution, obtains uniform mixing salt solution；
(2) n (OH-): n (Mg2++Al3+)=2: 1, n (Al3+): n (C2H5OCS2-)=1: 1 is pressed, is weighed a certain amount of
NaOH and sodium ethylxanthate (C2H5OCS2Na) add 100ml deionized water to make it completely dissolved in beaker, obtain uniform
Mixed ammonium/alkali solutions；
(3) take two air-tightness good, the identical constant pressure funnel of specification is cleaned, drying, and salt-mixture, aqueous slkali are distinguished
It is transferred in constant pressure funnel；
(4) salt-mixture, the aqueous slkali in constant pressure funnel are slowly dropped in beaker and are at the uniform velocity stirred, adjust rate of titration
The pH of reaction system is set to be consistently greater than 10；
(5) continue to stir 2h at room temperature after being added dropwise；
(6) it places the beaker in constant water bath box that crystallization is taken out after a certain period of time at a certain temperature after stirring, burns
Cup lower part is pale yellow precipitate；
(7) solution after ageing is filtered, and filter cake is washed with deionized to neutrality, 12h is dried at 80 DEG C；
(8) filter cake is taken out, grinding obtains pale yellow powder shape hydrotalcite, as ethoxy-dithioformic acid Intercalated.
Referring to Fig.1-3, ethoxy-dithioformic acid Intercalated produced by the present invention has better crystal structure.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (7)
1. a kind of method for preparing ethoxy-dithioformic acid Intercalated, it is characterised in that the following steps are included:
A, Aluminium chloride hexahydrate and Magnesium dichloride hexahydrate are weighed according to the ratio of molar ratio 2: 1, deionization is then added
It is dissolved in water, obtains mixed solution A；
B, urea and sodium ethylxanthate are weighed according to the ratio of molar ratio 4: 1, is then added in deionized water and carries out
Dissolution, obtains mixed solution B；
C, mixed solution B is placed in reaction vessel, mixed solution A is gradually added dropwise in mixed solution B, it is right at the same time
Mixed solution B is stirred, and 25 DEG C when the temperature in reaction vessel is by being added dropwise are linearly increasing to 75 that completion of dropwise addition is
DEG C, when mixed solution A is added dropwise to the 50% of its total amount, hydrogen-oxygen is added dropwise into mixed solution B while mixed solution A is added dropwise
Change sodium solution, the dropwise addition of sodium hydroxide solution and the dropwise addition of mixed solution A terminate simultaneously, the sodium hydroxide of dropwise addition and the urine of dropwise addition
The molar ratio of element is 1: 10；
D, accelerate mixing speed after being added dropwise, persistently stir 2h, be then allowed to stand 12h；
E, the solution after standing is filtered, and filter cake is washed with deionized to neutrality, dry 12h, takes out at 80 DEG C
Filter cake, grinding, obtains pale yellow powder shape hydrotalcite, as ethoxy-dithioformic acid Intercalated.
2. the method according to claim 1 for preparing ethoxy-dithioformic acid Intercalated, it is characterised in that: mixing is molten
In liquid A, the molar ratio of aluminium chloride and deionized water is 2: 25, in mixed solution B, mole of sodium ethylxanthate and deionized water
Than being 1: 40.
3. the method according to claim 2 for preparing ethoxy-dithioformic acid Intercalated, it is characterised in that: step C
In, mixing speed 120rad/min；In step D, mixing speed 350rad/min.
4. the method according to claim 3 for preparing ethoxy-dithioformic acid Intercalated, it is characterised in that: step D
In, solution temperature when standing is maintained at 40 DEG C.
5. the method according to claim 4 for preparing ethoxy-dithioformic acid Intercalated, it is characterised in that: step C
Nitrogen is filled in step D, in reaction vessel to be protected.
6. the method according to claim 1 for preparing ethoxy-dithioformic acid Intercalated, it is characterised in that: described anti-
Answering container includes cavity (1), and the bottom of cavity (1) is provided with inclined-plane (2), and the left-hand end of inclined-plane (2) is higher than right-hand end, inclined-plane
(2) it is equipped with above left-hand end drop tube (3), the end of drop tube (3) is connected with several dropwise addition heads arranged side by side
(4), agitating paddle (7) are installed above inclined-plane (2) right-hand end.
7. the method according to claim 6 for preparing ethoxy-dithioformic acid Intercalated, it is characterised in that: the drop
Add the side wall of pipe (3) to be equipped with primary heater (8), secondary heater (9) are installed in inclined-plane (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910158609.4A CN109734109B (en) | 2019-02-22 | 2019-02-22 | Method for preparing ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910158609.4A CN109734109B (en) | 2019-02-22 | 2019-02-22 | Method for preparing ethyl xanthic acid intercalated magnesium-aluminum hydrotalcite |
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| CN109734109A true CN109734109A (en) | 2019-05-10 |
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| US20140154165A1 (en) * | 2012-02-17 | 2014-06-05 | Beijing University Of Chemical Technology | Method for preparing graphene by using two-dimensional confined space between the layers of inorganic layered materials |
| CN108704603A (en) * | 2018-04-18 | 2018-10-26 | 中国科学院生态环境研究中心 | One step prepares method of the magnalium hydrotalcite nanometer sheet for adsorption and dephosphorization |
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2019
- 2019-02-22 CN CN201910158609.4A patent/CN109734109B/en not_active Expired - Fee Related
Patent Citations (6)
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| CN101293676A (en) * | 2008-06-12 | 2008-10-29 | 华东理工大学 | High-specific surface area nano-middle hole cobalt system spinel material and preparing method thereof |
| CN101530621A (en) * | 2009-03-18 | 2009-09-16 | 北京化工大学 | Oxidation resisting dipeptide medicament intercalated houghite and preparation method thereof |
| US20140154165A1 (en) * | 2012-02-17 | 2014-06-05 | Beijing University Of Chemical Technology | Method for preparing graphene by using two-dimensional confined space between the layers of inorganic layered materials |
| CN102796280A (en) * | 2012-08-29 | 2012-11-28 | 北京化工大学 | Supramolecular intercalated structure polymer antioxidant |
| CN103508638A (en) * | 2013-10-15 | 2014-01-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Combined wastewater treatment method through visible light catalysis and immobilized microorganisms and combined reactor |
| CN108704603A (en) * | 2018-04-18 | 2018-10-26 | 中国科学院生态环境研究中心 | One step prepares method of the magnalium hydrotalcite nanometer sheet for adsorption and dephosphorization |
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