CN109928521A - Inorganic microparticle scale dispersing agent and preparation method thereof - Google Patents
Inorganic microparticle scale dispersing agent and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of inorganic microparticle scale dispersing agent, sulfonation, silylating reagent are passed through by carbon nanotube, are prepared modified carbon nano-tube, modified carbon nano-tube again with ferroso-ferric oxide is compound obtains inorganic microparticle scale dispersing agent.The inorganic microparticle scale dispersing agent is non-corrosive to equipment, is insoluble in water, easily separated, and it is not phosphorous, it is environmentally protective on effect water quality without influence, scale inhibition effect is good, and compared to the blank group that scale dispersing agent is not added, this product, which is added, can be effectively suppressed the generation of equipment inner wall scale.The present invention also provides the preparation methods of above-mentioned inorganic microparticle scale dispersing agent, and preparation method is simple, can be with industrialized production.Inorganic microparticle scale dispersing agent of the present invention can be used for steamer cooling water recirculation system, and scale is prevented to be formed in heat exchanger surface and circulating line inner wall.
Description
Technical field
The present invention relates to a kind of scale dispersing agents, disperse more particularly to a kind of environmental type inorganic microparticle scale
Agent.
Background technique
Currently, scale dispersing agent is mostly soluble sour (phosphoric acid, phosphate), organic phosphine etc., have to acting device certain
Corrosivity, similar product are soluble acid or phosphorous polymer, and latency environment harm is larger.It is therefore desirable to research and develop one
Environmentally protective, the small scale dispersing agent of corrosivity of kind.
Summary of the invention
The purpose of the present invention is develop a kind of with environmentally protective inorganic microparticle water in view of the deficiencies of the prior art
Dirty dispersing agent.
The present invention provides a kind of inorganic microparticle scale dispersing agents, pass through sulfonation, silylating reagent, system by carbon nanotube
It is standby to obtain modified carbon nano-tube, modified carbon nano-tube again with ferroso-ferric oxide is compound obtains inorganic microparticle scale dispersing agent.
Further, the partial size of the inorganic microparticle scale dispersing agent is 0.05-0.5 μm.
Further, with XRD diagram as shown in Figure 1.
Further, with scanning electron microscope (SEM) photograph as shown in Figure 2.
Further, the carbon nanotube sulfonation is to use to react under carbon nanotube and concentrated sulfuric acid heating condition to be prepared
Sulfonated carbon nanotube, wherein the mass ratio of carbon nanotube and the concentrated sulfuric acid is 1:100-150, and heating reaction temperature is 120-160 DEG C.
Further, the modified carbon nano-tube is to react to obtain with amino silicane coupling agent by the carbon nanotube of sulfonation,
Wherein amino silicane coupling agent is a kind of in KH792, KH591, KH550, KH550 be gamma-aminopropyl-triethoxy-silane,
KH792 is γ-aminoethyl amino propyl trimethoxy silane, KH591 is N- aminoethyl-gamma-aminopropyl-triethoxy-silane.
Further, the modified carbon nano-tube is to react to obtain with amino silicane coupling agent by the carbon nanotube of sulfonation,
Specifically, amino silicane coupling agent is added in the mixed solution of second alcohol and water, stirring hydrolysis obtains solution, then into solution
Sulfonated carbon nanotube is added, stirring, 40-60 DEG C of temperature, 1-2 hour of reaction time, filtering, filter cake is wash with distilled water to pH
=6.5-7.0, is dried to obtain modified carbon nano-tube；Wherein, the volume mass of amino silicane coupling agent and Sulfonated carbon nanotube ratio
It (mL/g) is 0.02-0.05:1, amino silicane coupling agent: water: ethyl alcohol volume ratio is 1-5- 10:90.
Further, modified carbon nano-tube and ferroso-ferric oxide Combined Mining be using the following method:
Modified carbon nano-tube reacts to obtain carbon nanotube ferriferrous oxide composite material with iron salt solutions；
The wherein preparation of iron salt solutions are as follows: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution,
Stir evenly, ferric chloride (FeCl36H2O), sodium acetate, ethylene glycol, polyethylene glycol mass ratio be 1:8-10:20-30:0.8-1.2, gather
The molecular weight of ethylene glycol is 2000-4000.
Further, iron salt solutions move into hydrothermal reaction kettle, and modified carbon nano-tube is added, and react 10-16 hours, reaction temperature
120-160 DEG C of degree, end of reaction is cooled to room temperature, and takes out filtering, is cleaned and dried；Product after drying is put into sintering furnace,
200-250 DEG C of sintering, 5 DEG C/min of heating rate keep the temperature 2-4 hours, take out, and grinding obtains final products inorganic microparticle water
Dirty dispersing agent, wherein the mass ratio of ferric chloride (FeCl36H2O) and modified carbon nano-tube is 1:0.05-0.1.
The present invention also provides the preparation methods of above-mentioned inorganic microparticle scale dispersing agent, include the following steps:
Sulfonating reaction occurs for the first step, carbon nanotube and the concentrated sulfuric acid, obtains Sulfonated carbon nanotube；
Second step, Sulfonated carbon nanotube react to obtain modified carbon nano-tube with amino silicane coupling agent；
Third step, modified carbon nano-tube with ferroso-ferric oxide is compound obtains inorganic microparticle scale dispersing agent.
Further, the preparation method of above-mentioned inorganic microparticle scale dispersing agent, comprising the following steps:
Step 1: the concentrated sulfuric acid is added in carbon nanotube, the volume mass ratio (mL/g) of the concentrated sulfuric acid and carbon nanotube is 100-
150:1, reflux time 12-30 hours, is cooled to room temperature, is diluted with water by 120-160 DEG C of reaction temperature, filtering, water cleaning
Filter cake is dried to obtain Sulfonated carbon nanotube to pH=6.5-7.0；
Step 2: amino silicane coupling agent is added in the mixed solution of second alcohol and water, stirring hydrolysis obtains solution；To above-mentioned
A certain amount of Sulfonated carbon nanotube is added in solution, stirs, 40-60 DEG C of temperature, 1-2 hour of reaction time, filtering, filter cake is used
Distilled water is cleaned to pH=6.5-7.0, is dried to obtain modified carbon nano-tube；Wherein, silane coupling agent: water: ethyl alcohol volume ratio is 1-
The volume mass ratio (mL/g) of 5-10:90, amino silicane coupling agent and Sulfonated carbon nanotube is 20-50:1；
Step 3: the preparation of carbon nanotube ferriferrous oxide composite material:
1. the preparation of iron salt solutions: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution, stirring
Uniformly, ferric chloride (FeCl36H2O), sodium acetate, ethylene glycol, polyethylene glycol mass ratio be 1:8-10:20-30:0.8-1.2, poly- second two
The molecular weight of alcohol is 2000-4000；
2. hydro-thermal reaction prepares composite material: above-mentioned solution is moved into hydrothermal reaction kettle, addition and modified carbon nano-tube, reaction
10-16 hours, 120-160 DEG C of reaction temperature, end of reaction was cooled to room temperature, and took out filtering, was cleaned and dried, wherein six water three
The mass ratio of iron chloride and modified carbon nano-tube is 1:0.05-0.1；
3. the preparation of carbon nanotube ferriferrous oxide composite material: the product after drying being put into sintering furnace, 200-250 DEG C of burning
Knot, 5 DEG C/min of heating rate keep the temperature 2-4 hours, take out, and grinding obtains final products inorganic microparticle scale dispersing agent.
The present invention also provides the purposes of above-mentioned inorganic microparticle scale dispersing agent, which can
For steamer cooling water recirculation system, scale is prevented to be formed in heat exchanger surface and circulating line inner wall.
Compared with the prior art, the invention has the following advantages:
1, inorganic microparticle scale dispersing agent provided by the invention is non-corrosive to equipment, is insoluble in water, easily separated, and is free of
Phosphorus, it is environmentally protective on effect water quality without influence.
2, inorganic microparticle scale dispersing agent scale inhibition effect provided by the invention is good, compared to the sky that scale dispersing agent is not added
White group, hence it is evident that reduce scale and generate.
3, inorganic microparticle scale dispersant preparation method provided by the invention is simple, can be with industrialized production.
Detailed description of the invention
Fig. 1 is the XPD powder diagram for the inorganic microparticle scale dispersing agent that the embodiment of the present invention 1 provides；
Fig. 2 is the scanning electron microscope (SEM) photograph for the inorganic microparticle scale dispersing agent that the embodiment of the present invention 1 provides.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
The measurement of X ray powder diffraction (XPD) is using Panalytical Empyrean X ray powder diffraction
Analyzer carries out.
Embodiment 1
Step 1: carbon nanotube sulfonation
Sulfuric acid is to carbon nanotube sulfonation modifying: concentrated sulfuric acid 1.2L is added in 10g carbon nanotube, and 140 DEG C of reaction temperature, reflux is anti-
It 30 hours between seasonable, is cooled to room temperature, distilled water dilution, filtering, distilled water cleans filter cake to pH=7, vacuum drying；
Step 2: the silanization of Sulfonated carbon nanotube
Amino silicane coupling agent hydrolysis: amino silicane coupling agent (KH792) is added in the mixed solution of second alcohol and water, silane
Coupling agent: water: ethyl alcohol volume ratio be 1:10:90,1 hour of hydrolysis time, 40 DEG C of hydrolysis temperature；
Silane coupling agent is to carbon nano-tube modification: corresponding to 0.02g Sulfonated carbon nanotube according to every mL amino silicane coupling agent, upwards
It states and Sulfonated carbon nanotube is added in solution, magnetic agitation, temperature 60 C, 1 hour of reaction time, filtering, filter cake distilled water
Cleaning to pH=7, vacuum drying obtains modified carbon nano-tube；
Step 3: the preparation of carbon nanotube ferriferrous oxide composite material:
1, the preparation of iron salt solutions: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution, stirring
Uniformly, ferric chloride (FeCl36H2O), sodium acetate the ratio of amount of substance be 1:8, ethylene glycol makees solvent, and dosage is tri-chlorination irony
20 times of amount, polyethylene glycol (molecular weight 2000), dosage are 1.2 times of ferric trichloride quality；
2, hydro-thermal reaction prepares composite material: above-mentioned solution being moved into hydrothermal reaction kettle, addition is with ferric trichloride mass ratio
0.05 times of modified carbon nano-tube reacts 12 hours, and 140 DEG C of reaction temperature, end of reaction is cooled to room temperature, and takes out filtering, clearly
Wash drying；
3, the preparation of carbon nanotube ferriferrous oxide composite material: the product after drying is put into sintering furnace, 250 DEG C of sintering,
5 DEG C/min of heating rate keeps the temperature 4 hours, takes out, and grinding obtains final products inorganic microparticle scale dispersing agent, using laser
Its particle size of particle size analyzer determination is 0.1 μm.X-ray powder measurement is carried out using Cu-ka ray, is had as shown in Figure 1
Map.Using scanning electron microscopic observation, appearance shown in Fig. 2.
Embodiment 2
Step 1: carbon nanotube sulfonation
Sulfuric acid is to carbon nanotube sulfonation modifying: concentrated sulfuric acid 1L is added in 10g carbon nanotube, and 120 DEG C of reaction temperature, back flow reaction
It time 12 hours, is cooled to room temperature, distilled water dilution, filtering, distilled water cleans filter cake to pH=7, vacuum drying；
Step 2: the silanization of Sulfonated carbon nanotube
Amino silicane coupling agent hydrolysis: amino silicane coupling agent (KH591) is added in the mixed solution of second alcohol and water, silane
Coupling agent: water: ethyl alcohol volume ratio be 1:5:90,2 hours of hydrolysis time, 50 DEG C of hydrolysis temperature；
Silane coupling agent is to carbon nano-tube modification: corresponding to 0.05g Sulfonated carbon nanotube according to every mL amino silicane coupling agent, upwards
It states and Sulfonated carbon nanotube is added in solution, magnetic agitation, temperature 60 C, 1 hour of reaction time, filtering, filter cake distilled water
Cleaning to pH=7, vacuum drying obtains modified carbon nano-tube；
Step 3: the preparation of carbon nanotube ferriferrous oxide composite material:
1, the preparation of iron salt solutions: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution, stirring
Uniformly, ferric chloride (FeCl36H2O), sodium acetate the ratio of amount of substance be 1:10, ethylene glycol makees solvent, and dosage is ferric trichloride
20 times of quality, polyethylene glycol (molecular weight 4000), dosage are 0.8 times of ferric trichloride quality；
2, hydro-thermal reaction prepares composite material: above-mentioned solution being moved into hydrothermal reaction kettle, addition is with ferric trichloride mass ratio
0.05 times of modified carbon nano-tube reacts 16 hours, and 120 DEG C of reaction temperature, end of reaction is cooled to room temperature, and takes out filtering, clearly
Wash drying；
3, the preparation of carbon nanotube ferriferrous oxide composite material: the product after drying is put into sintering furnace, 250 DEG C of sintering,
5 DEG C/min of heating rate keeps the temperature 4 hours, takes out, and grinding obtains final products inorganic microparticle scale dispersing agent.
Embodiment 3
Step 1: carbon nanotube sulfonation
Sulfuric acid is to carbon nanotube sulfonation modifying: concentrated sulfuric acid 1L is added in 10g carbon nanotube, and 120 DEG C of reaction temperature, back flow reaction
It time 12 hours, is cooled to room temperature, distilled water dilution, filtering, distilled water cleans filter cake to pH=7, vacuum drying；
Step 2: the silanization of Sulfonated carbon nanotube
Amino silicane coupling agent hydrolysis: amino silicane coupling agent (KH550) is added in the mixed solution of second alcohol and water, silane
Coupling agent: water: ethyl alcohol volume ratio be 1:8:90,2 hours of hydrolysis time, 60 DEG C of hydrolysis temperature；
Silane coupling agent is to carbon nano-tube modification: corresponding to 0.05g Sulfonated carbon nanotube according to every mL amino silicane coupling agent, upwards
It states and Sulfonated carbon nanotube is added in solution, magnetic agitation, temperature 60 C, 1 hour of reaction time, filtering, filter cake distilled water
Cleaning to pH=7, vacuum drying obtains modified carbon nano-tube；
Step 3: the preparation of carbon nanotube ferriferrous oxide composite material:
1, the preparation of iron salt solutions: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution, stirring
Uniformly, ferric chloride (FeCl36H2O), sodium acetate the ratio of amount of substance be 1:8, ethylene glycol makees solvent, and dosage is tri-chlorination irony
30 times of amount, polyethylene glycol (molecular weight 2000), dosage are 1.0 times of ferric trichloride quality；
2, hydro-thermal reaction prepares composite material: above-mentioned solution being moved into hydrothermal reaction kettle, being added with ferric trichloride mass ratio is 0.1
Modified carbon nano-tube again reacts 10 hours, and 120 DEG C of reaction temperature, end of reaction is cooled to room temperature, and takes out filtering, and cleaning is done
It is dry；
3, the preparation of carbon nanotube ferriferrous oxide composite material: the product after drying is put into sintering furnace, 250 DEG C of sintering,
5 DEG C/min of heating rate keeps the temperature 4 hours, takes out, and grinding obtains final products inorganic microparticle scale dispersing agent.
Embodiment 4
Sulfuric acid is to carbon nanotube sulfonation modifying: concentrated sulfuric acid 1.5L is added in 10g carbon nanotube, and 160 DEG C of reaction temperature, reflux is anti-
It 20 hours between seasonable, is cooled to room temperature, distilled water dilution, filtering, distilled water cleans filter cake to pH=7, vacuum drying；
Step 2: the silanization of Sulfonated carbon nanotube
Amino silicane coupling agent hydrolysis: amino silicane coupling agent (KH550) is added in the mixed solution of second alcohol and water, silane
Coupling agent: water: ethyl alcohol volume ratio be 1:5:90,2 hours of hydrolysis time, 60 DEG C of hydrolysis temperature；
Silane coupling agent is to carbon nano-tube modification: corresponding to 0.03g Sulfonated carbon nanotube according to every mL amino silicane coupling agent, upwards
It states and Sulfonated carbon nanotube is added in solution, magnetic agitation, 40 DEG C of temperature, 2 hours of reaction time, filtering, filter cake distilled water
Cleaning to pH=7, vacuum drying obtains modified carbon nano-tube；
Step 3: the preparation of carbon nanotube ferriferrous oxide composite material:
1, the preparation of iron salt solutions: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution, stirring
Uniformly, ferric chloride (FeCl36H2O), sodium acetate the ratio of amount of substance be 1:9, ethylene glycol makees solvent, and dosage is tri-chlorination irony
25 times of amount, polyethylene glycol (molecular weight 4000), dosage are 1.2 times of ferric trichloride quality；
2, hydro-thermal reaction prepares composite material: above-mentioned solution being moved into hydrothermal reaction kettle, addition is with ferric trichloride mass ratio
0.07 times of modified carbon nano-tube reacts 16 hours, and 160 DEG C of reaction temperature, end of reaction is cooled to room temperature, and takes out filtering, clearly
Wash drying；
3, the preparation of carbon nanotube ferriferrous oxide composite material: the product after drying is put into sintering furnace, 250 DEG C of sintering,
5 DEG C/min of heating rate keeps the temperature 4 hours, takes out, and grinding obtains final products inorganic microparticle scale dispersing agent.
The effect of inorganic microparticle scale dispersing agent of the present invention is verified below by way of experimental example 1 and 2.
Test example 1
Using 304 stainless steel lacing films as test sample, it is dipped into 60 DEG C of inorganic microparticles that the offer of the embodiment of the present invention 1 is provided
In the originally water circulation system of scale dispersing agent, dosage 0.01g/L, and the tap water of product of the present invention is not added with another group
The circulatory system is done blank control and is taken out stainless steel lacing film and clear with deionized water after two groups of circulations are run 30 days
It washes, dry weighing increases judgement sample surface scale degree according to example weight.The gain in weight of blank group lacing film is 0.385g,
The lacing film gain in weight that the inorganic microparticle scale dispersing agent group that the embodiment of the present invention 1 provides is added is only 0.080g, sample weight gain
Quality and blank reduce 80% or so.
Test example 2
Using 304 stainless steel lacing films as test sample, it is dipped into 60 DEG C of inorganic microparticles that the offer of the embodiment of the present invention 1 is provided
In the originally water circulation system of scale dispersing agent, dosage 0.02g/L, and this product of the present invention is not added originally with another group
Water circulation system does blank control and takes out stainless steel lacing film after two groups of circulations are run 30 days and use deionized water
Cleaning, dry weighing increase judgement sample surface scale degree according to example weight.The gain in weight of blank group lacing film is
0.385g, the lacing film gain in weight that the inorganic microparticle scale dispersing agent group that the embodiment of the present invention 1 provides is added is only 0.030g, sample
Product weight gain quality and blank, reduce 90% or more.
By test example 1 and 2 it is found that inorganic microparticle scale dispersing agent scale inhibition effect is good, compared to scale dispersing agent is not added
Blank group, hence it is evident that reduce scale generate.
To sum up, inorganic microparticle scale dispersing agent provided by the invention is non-corrosive to equipment, is insoluble in water, easily separated,
And it is not phosphorous, on effect water quality without influence, environmentally protective, scale inhibition effect is good, compared to the blank that scale dispersing agent is not added
Group, this product, which is added, can be effectively suppressed the generation of equipment inner wall scale.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of inorganic microparticle scale dispersing agent, it is characterised in that: pass through sulfonation, silylating reagent, preparation by carbon nanotube
Obtain modified carbon nano-tube, modified carbon nano-tube again with ferroso-ferric oxide is compound obtains inorganic microparticle scale dispersing agent.
2. inorganic microparticle scale dispersing agent according to claim 1, it is characterised in that: the inorganic microparticle scale point
The partial size of powder is 0.05-0.5 μm；Preferably, with XRD diagram as shown in Figure 1；Preferably, have as shown in Figure 2
Scanning electron microscope (SEM) photograph.
3. inorganic microparticle scale dispersing agent according to claim 1, it is characterised in that: the carbon nanotube sulfonation is to adopt
Sulfonated carbon nanotube is prepared with reacting under carbon nanotube and concentrated sulfuric acid heating condition, wherein the matter of carbon nanotube and the concentrated sulfuric acid
Measuring volume ratio (g/mL) is 1:100-150, and heating reaction temperature is 120-160 DEG C.
4. inorganic microparticle scale dispersing agent according to claim 1, it is characterised in that: the modified carbon nano-tube is will
The carbon nanotube of sulfonation reacts to obtain with amino silicane coupling agent, wherein amino silicane coupling agent be selected from KH792, KH591,
It is a kind of in KH550.
5. inorganic microparticle scale dispersing agent according to claim 4, it is characterised in that: amino silicane coupling agent to be added
Into the mixed solution of second alcohol and water, stirring hydrolysis obtains solution, then Sulfonated carbon nanotube is added into solution, stirs, temperature
It 40-60 DEG C, 1-2 hour of reaction time, filters, filter cake to pH=6.5-7.0, is dried to obtain carbon modified and receives wash with distilled water
Mitron；Wherein, the volume mass of amino silicane coupling agent and Sulfonated carbon nanotube ratio (mL/g) is 0.02-0.05:1, amino silicone
Alkane coupling agent: water: ethyl alcohol volume ratio is 1-5-10:90.
6. inorganic microparticle scale dispersing agent according to claim 1, it is characterised in that: modified carbon nano-tube and four oxidations
Three-iron Combined Mining is using the following method:
Modified carbon nano-tube reacts to obtain carbon nanotube ferriferrous oxide composite material with iron salt solutions；
The wherein preparation of iron salt solutions are as follows: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution,
Stir evenly, ferric chloride (FeCl36H2O), sodium acetate, ethylene glycol, polyethylene glycol mass ratio be 1:8-10:20-30:0.8-1.2, gather
The molecular weight of ethylene glycol is 2000-4000.
7. inorganic microparticle scale dispersing agent according to claim 6, it is characterised in that:
Iron salt solutions immigration hydrothermal reaction kettle, addition modified carbon nano-tube, reaction 10-16 hours, 120-160 DEG C of reaction temperature,
End of reaction is cooled to room temperature, and takes out filtering, is cleaned and dried；Product after drying is put into sintering furnace, 200-250 DEG C of burning
Knot, 5 DEG C/min of heating rate keep the temperature 2-4 hours, take out, and grinding obtains final products inorganic microparticle scale dispersing agent,
The mass ratio of middle ferric chloride (FeCl36H2O) and modified carbon nano-tube is 1:0.05-0.1.
8. the preparation method of inorganic microparticle scale dispersing agent described in a kind of claim 1-7, it is characterised in that: including as follows
Step:
(a) sulfonating reaction occurs for carbon nanotube and the concentrated sulfuric acid, obtains Sulfonated carbon nanotube；
(b) Sulfonated carbon nanotube reacts to obtain modified carbon nano-tube with amino silicane coupling agent；
(c) modified carbon nano-tube with ferroso-ferric oxide is compound obtains inorganic microparticle scale dispersing agent.
9. the preparation method of inorganic microparticle scale dispersing agent according to claim 8, it is characterised in that: including following step
It is rapid:
Step 1: the concentrated sulfuric acid is added in carbon nanotube, the volume mass ratio (mL/g) of the concentrated sulfuric acid and carbon nanotube is 100-
150:1, reflux time 12-30 hours, is cooled to room temperature, is diluted with water by 120-160 DEG C of reaction temperature, filtering, water cleaning
Filter cake is dried to obtain Sulfonated carbon nanotube to pH=6.5-7.0；
Step 2: amino silicane coupling agent is added in the mixed solution of second alcohol and water, stirring hydrolysis obtains solution；To above-mentioned
A certain amount of Sulfonated carbon nanotube is added in solution, stirs, 40-60 DEG C of temperature, 1-2 hour of reaction time, filtering, filter cake is used
Distilled water is cleaned to pH=6.5-7.0, is dried to obtain modified carbon nano-tube；Wherein, silane coupling agent: water: ethyl alcohol volume ratio is 1-
The volume mass ratio (mL/g) of 5-10:90, amino silicane coupling agent and Sulfonated carbon nanotube is 20-50:1；
Step 3: the preparation of carbon nanotube ferriferrous oxide composite material:
1. the preparation of iron salt solutions: by ferric chloride (FeCl36H2O), anhydrous sodium acetate, polyethylene glycol is dissolved in ethylene glycol solution, stirring
Uniformly, ferric chloride (FeCl36H2O), sodium acetate, ethylene glycol, polyethylene glycol mass ratio be 1:8-10:20-30:0.8-1.2, poly- second two
The molecular weight of alcohol is 2000-4000；
2. hydro-thermal reaction prepares composite material: above-mentioned solution is moved into hydrothermal reaction kettle, addition and modified carbon nano-tube, reaction
10-16 hours, 120-160 DEG C of reaction temperature, end of reaction was cooled to room temperature, and took out filtering, was cleaned and dried, wherein six water three
The mass ratio of iron chloride and modified carbon nano-tube is 1:0.05-0.1；
3. the preparation of carbon nanotube ferriferrous oxide composite material: the product after drying being put into sintering furnace, 200-250 DEG C of burning
Knot, 5 DEG C/min of heating rate keep the temperature 2-4 hours, take out, and grinding obtains final products inorganic microparticle scale dispersing agent.
10. inorganic microparticle scale dispersing agent according to claim 1, it is characterised in that: the inorganic microparticle scale point
Powder can be used for steamer cooling water recirculation system.
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| 上海海运学院轮机系辅机教研组编: "《船舶辅机 （一） 船舶辅助锅炉与海水淡化装置》", 31 December 1977, 上海海运学院 * |
| 贾颖等编: "《轻质碳材料的应用》", 30 November 2013, 国防工业出版社 * |
| 黄涛，张秋生主编: "《锅炉压力容器十大技术标准规范 锅炉用水处理技术标准》", 31 May 2005, 北京科技大学电子出版社 * |
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