CN110127864A - Compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water and preparation method thereof - Google Patents
Compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water and preparation method thereof Download PDFInfo
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- CN110127864A CN110127864A CN201910482416.4A CN201910482416A CN110127864A CN 110127864 A CN110127864 A CN 110127864A CN 201910482416 A CN201910482416 A CN 201910482416A CN 110127864 A CN110127864 A CN 110127864A
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- fullerene
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
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Abstract
The invention discloses compound scale dispersing agents of the inorganic particle of a kind of Domestic floor recirculated water and preparation method thereof, fullerene is taken to be added in sulfuric acid first, it is stirred at reflux, add nitric acid, filtering, it is dried in vacuo to obtain acidification fullerene, acidification fullerene is distributed in dimethylformamide, instill thionyl chloride, the reaction was continued, tetrahydrofuran is added, centrifuge separation, vacuum drying obtains chloride fullerene, chloride fullerene is added in diamine, condensing agent is added, and the reaction was continued, washing, filtering, it is dried in vacuo to obtain amination fullerene, then ferric trichloride is taken, anhydrous sodium acetate and hexamethylene diamine are dissolved in ethylene glycol solution, it stirs evenly, amination fullerene is added to be reacted, filtering, cleaning, it is dry, sintering, grinding, obtain amination fullerene ferric oxide composite material.Preparation process of the invention is simple, can be with industrialized production, and the scale dispersing agent prepared is non-corrosive to equipment and not phosphorous, environmentally protective on environment without influence.
Description
Technical field
The present invention relates to water treatment agent technical fields, compound more particularly to a kind of inorganic particle of Domestic floor recirculated water
Scale dispersing agent and preparation method thereof.
Background technique
The dirt of circulation not only will affect heat-transfer effect, can also cause to corrode cooperating microorganisms indirectly and cause defeated
Water is difficult.Common scale removal or method of scale inhibition mainly include two classes in Domestic floor at present: physical scale inhibition method and chemical scale-inhibiting
Method.Wherein, chemical scale-inhibitor is P containing sludge inhibitor, is broadly divided into four kinds: Quadrafos, organic phospho acid, organic phosphine carboxylic acid and
Phosphinocarboxylic acid, however most of P containing sludge inhibitors can all cause different degrees of pollution to environment, be badly in need of at present a kind of without phosphorus
(phosphine) inorganic inhibitors.
Summary of the invention
To solve problems of the prior art, it is multiple that the present invention provides a kind of inorganic particles of Domestic floor recirculated water
Heshui dirt dispersing agent and preparation method thereof, simple process can be with industrialized production, and the scale dispersing agent of preparation is to effect water body
Water quality is without influence, easily separated, no environmental protection pressure.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, including following raw material: fullerene, protochloride
Sulfone, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous sodium acetate, hexamethylene diamine.
Preferably, the mass ratio of the fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide are as follows:
Fullerene: thionyl chloride: diamine: dicyclohexylcarbodiimide=1:3.5~13:0.08~3.2:15~20.
Preferably, the molar ratio of the anhydrous sodium acetate, ferric trichloride are as follows:
Anhydrous sodium acetate: ferric trichloride=6~9:1；
The mass ratio of the hexamethylene diamine, ferric trichloride are as follows:
Hexamethylene diamine: ferric trichloride=5~7:1；
The molar ratio of the fullerene, ferric trichloride:
Fullerene: ferric trichloride=2~5:1.
The present invention also provides a kind of preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water,
Technical solution is:
A kind of preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, comprising the following steps:
S1, amination modified fullerene；
S2, preparation amination fullerene ferric oxide composite material.
Preferably, step S1 specifically includes the following steps:
S11, take fullerene be added sulfuric acid in, control reaction temperature be 90 DEG C~120 DEG C, be stirred at reflux, react for 6h~
12h；
S12, nitric acid is added, control reaction temperature is 70 DEG C~90 DEG C, is stirred at reflux, and the reaction time is 12h~for 24 hours；
S13, it is cooled to room temperature, filters, it is 6.5~7.0 that deionized water, which is washed to pH, is dried in vacuo to obtain acidification fullerene；
S14, acidification fullerene is distributed in solvent dimethylformamide, instills thionyl chloride, is uniformly mixed；
S15, control reaction temperature are 60 DEG C~70 DEG C, are stirred at reflux for 24 hours~36h；
S16, tetrahydrofuran solvent, centrifuge separation is added, vacuum drying obtains chloride fullerene；
S17, chloride fullerene is added in binary amine solvent, dicyclohexylcarbodiimide, control reaction temperature is added
Degree is 130 DEG C~160 DEG C, is stirred at reflux for 24 hours~48h；
S18, dehydrated alcohol, supersound washing is added, filtering is dried in vacuo to obtain amination fullerene.
Preferably, the mass ratio of fullerene described in step S11 and sulfuric acid is 1:75~137.
Preferably, the volume ratio of nitric acid described in step S12 and sulfuric acid described in step S11 is 1~1.5:1.
Preferably, the volume ratio of tetrahydrofuran described in step S16 and thionyl chloride described in step S14 is 20~30:
1。
Preferably, diamine described in step S17 is one or more of ethylenediamine, hexamethylene diamine and decamethylene diamine.
Preferably, step S2 specifically includes the following steps:
S21, take ferric trichloride, anhydrous sodium acetate and hexamethylene diamine be dissolved in in, controlled at 70 DEG C~80 DEG C, stirring is equal
It is even；
S22, amination fullerene is added, control reaction temperature is 120 DEG C~160 DEG C, reacts 8h~12h, is cooled to room
Temperature is taken out filtering, is successively cleaned with water and ethyl alcohol, dry；
S23, control heating rate are 3 DEG C/min, and in 150 DEG C~230 DEG C heat preservation sintering 1h~2h, grinding obtains amination
Fullerene ferric oxide composite material.
The beneficial effects of the present invention are:
1, inorganic particle scale dispersant preparation method provided by the invention is simple, can be with industrialized production.
2, inorganic particle scale dispersing agent scale inhibition effect prepared by the present invention is good, compared to the blank that scale dispersing agent is not added
Group, hence it is evident that reduce scale and generate.
3, inorganic particle scale dispersing agent prepared by the present invention is non-corrosive to equipment, and not phosphorous, on environment without influence,
It is environmentally protective.
4, inorganic particle scale dispersing agent prepared by the present invention is on effect water quality without influence, easily separated, acyclic pressure maintaining
Power.
Specific embodiment
The embodiment of the present invention is described in detail below.
Embodiment 1
A kind of compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, including following raw material: fullerene, protochloride
Sulfone, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous sodium acetate, hexamethylene diamine.
Wherein, the mass ratio of fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide are as follows:
Fullerene: thionyl chloride: diamine: dicyclohexylcarbodiimide=1:3.5:0.08:15；
The molar ratio of anhydrous sodium acetate, ferric trichloride are as follows:
Anhydrous sodium acetate: ferric trichloride=6:1；
The mass ratio of hexamethylene diamine, ferric trichloride are as follows:
Hexamethylene diamine: ferric trichloride=5:1；
The molar ratio of fullerene, ferric trichloride:
Fullerene: ferric trichloride=2:1.
Embodiment 2
A kind of compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, including following raw material: fullerene, protochloride
Sulfone, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous sodium acetate, hexamethylene diamine.
Wherein, the mass ratio of fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide are as follows:
Fullerene: thionyl chloride: diamine: dicyclohexylcarbodiimide=1:13:3.2:20；
The molar ratio of anhydrous sodium acetate, ferric trichloride are as follows:
Anhydrous sodium acetate: ferric trichloride=9:1；
The mass ratio of hexamethylene diamine, ferric trichloride are as follows:
Hexamethylene diamine: ferric trichloride=7:1；
The molar ratio of fullerene, ferric trichloride:
Fullerene: ferric trichloride=5:1.
Embodiment 3
A kind of compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, including following raw material: fullerene, protochloride
Sulfone, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous sodium acetate, hexamethylene diamine.
Wherein, the mass ratio of fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide are as follows:
Fullerene: thionyl chloride: diamine: dicyclohexylcarbodiimide=1:10:2.4:18；
The molar ratio of anhydrous sodium acetate, ferric trichloride are as follows:
Anhydrous sodium acetate: ferric trichloride=7:1；
The mass ratio of hexamethylene diamine, ferric trichloride are as follows:
Hexamethylene diamine: ferric trichloride=6:1；
The molar ratio of fullerene, ferric trichloride:
Fullerene: ferric trichloride=4:1.
Embodiment 4
A kind of preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, comprising the following steps:
(1) amination modified fullerene:
S11, fullerene is taken to be added in sulfuric acid, the mass ratio of fullerene and sulfuric acid is 1:75, and control reaction temperature is 90 DEG C,
It is stirred at reflux, reacts for 6h；
The volume ratio of S12, addition nitric acid, nitric acid and sulfuric acid is 1:1, and control reaction temperature is 70 DEG C, is stirred at reflux, reacts
Time is 12h；
S13, it is cooled to room temperature, filters, it is 6.5 that deionized water, which is washed to pH, is dried in vacuo to obtain acidification fullerene；
S14, acidification fullerene is distributed in solvent dimethylformamide, instills thionyl chloride, is uniformly mixed；
S15, control reaction temperature are 60 DEG C, are stirred at reflux for 24 hours；
The volume ratio of S16, addition tetrahydrofuran solvent, tetrahydrofuran and thionyl chloride is 20:1, is centrifugated, vacuum is dry
It is dry to obtain chloride fullerene；
S17, chloride fullerene is added in ethylenediamine solvent, dicyclohexylcarbodiimide, control reaction temperature is added
Degree is 130 DEG C, is stirred at reflux for 24 hours；
S18, dehydrated alcohol, supersound washing is added, filtering is dried in vacuo to obtain amination fullerene.
(2) amination fullerene ferric oxide composite material is prepared:
S21, it takes during ferric trichloride, anhydrous sodium acetate and hexamethylene diamine be dissolved in, controlled at 70 DEG C, stirs evenly；
S22, amination fullerene being added, control reaction temperature is 120 DEG C, 8h reacted, is cooled to room temperature, filtering is taken out,
Successively cleaned with water and ethyl alcohol, it is dry；
S23, control heating rate are 3 DEG C/min, and in 150 DEG C of heat preservation sintering 1h, grinding obtains the oxidation of amination fullerene three
Two iron composite materials.
Fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous acetic acid in the present embodiment
The proportion such as embodiment 1 of sodium, hexamethylene diamine.
Embodiment 5
A kind of preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, comprising the following steps:
(1) amination modified fullerene:
S11, fullerene is taken to be added in sulfuric acid, the mass ratio of fullerene and sulfuric acid is 1:137, and control reaction temperature is 120
DEG C, it is stirred at reflux, reacts for 12h；
The volume ratio of S12, addition nitric acid, nitric acid and sulfuric acid is 1.5:1, and control reaction temperature is 90 DEG C, is stirred at reflux, instead
For for 24 hours between seasonable；
S13, it is cooled to room temperature, filters, it is 7.0 that deionized water, which is washed to pH, is dried in vacuo to obtain acidification fullerene；
S14, acidification fullerene is distributed in solvent dimethylformamide, instills thionyl chloride, is uniformly mixed；
S15, control reaction temperature are 70 DEG C, are stirred at reflux 36h；
The volume ratio of S16, addition tetrahydrofuran solvent, tetrahydrofuran and thionyl chloride is 30:1, is centrifugated, vacuum is dry
It is dry to obtain chloride fullerene；
S17, chloride fullerene is added in hexamethylene diamine solvent, dicyclohexylcarbodiimide, control reaction temperature is added
Degree is 160 DEG C, is stirred at reflux 48h；
S18, dehydrated alcohol, supersound washing is added, filtering is dried in vacuo to obtain amination fullerene.
(2) amination fullerene ferric oxide composite material is prepared:
S21, it takes during ferric trichloride, anhydrous sodium acetate and hexamethylene diamine be dissolved in, controlled at 80 DEG C, stirs evenly；
S22, amination fullerene being added, control reaction temperature is 160 DEG C, 12h reacted, is cooled to room temperature, filtering is taken out,
Successively cleaned with water and ethyl alcohol, it is dry；
S23, control heating rate are 3 DEG C/min, and in 230 DEG C of heat preservation sintering 2h, grinding obtains the oxidation of amination fullerene three
Two iron composite materials.
Fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous acetic acid in the present embodiment
The proportion such as embodiment 2 of sodium, hexamethylene diamine.
Embodiment 6
A kind of preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, comprising the following steps:
(1) amination modified fullerene:
S11, fullerene is taken to be added in sulfuric acid, the mass ratio of fullerene and sulfuric acid is 1:100, and control reaction temperature is 100
DEG C, it is stirred at reflux, reacts for 8h；
The volume ratio of S12, addition nitric acid, nitric acid and sulfuric acid is 1.2:1, and control reaction temperature is 80 DEG C, is stirred at reflux, instead
It is 18h between seasonable；
S13, it is cooled to room temperature, filters, it is 7.0 that deionized water, which is washed to pH, is dried in vacuo to obtain acidification fullerene；
S14, acidification fullerene is distributed in solvent dimethylformamide, instills thionyl chloride, is uniformly mixed；
S15, control reaction temperature are 65 DEG C, are stirred at reflux 30h；
The volume ratio of S16, addition tetrahydrofuran solvent, tetrahydrofuran and thionyl chloride is 25:1, is centrifugated, vacuum is dry
It is dry to obtain chloride fullerene；
S17, chloride fullerene is added in decamethylene diamine solvent, dicyclohexylcarbodiimide, control reaction temperature is added
Degree is 140 DEG C, is stirred at reflux 36h；
S18, dehydrated alcohol, supersound washing is added, filtering is dried in vacuo to obtain amination fullerene.
(2) amination fullerene ferric oxide composite material is prepared:
S21, it takes during ferric trichloride, anhydrous sodium acetate and hexamethylene diamine be dissolved in, controlled at 75 DEG C, stirs evenly；
S22, amination fullerene being added, control reaction temperature is 140 DEG C, 10h reacted, is cooled to room temperature, filtering is taken out,
Successively cleaned with water and ethyl alcohol, it is dry；
S23, control heating rate are 3 DEG C/min, and in 200 DEG C of heat preservation sintering 1.5h, grinding obtains three oxygen of amination fullerene
Change two iron composite materials.
Fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous acetic acid in the present embodiment
The proportion such as embodiment 3 of sodium, hexamethylene diamine.
It is 100m to service area2Domestic floor system in the inorganic particle scale that provides in the embodiment of the present invention is provided
Dispersing agent, the water being added in ground heating system are tap water, and the dosage of inorganic particle scale dispersing agent is 0.1g/L, not with 304
Rust steel lacing film is placed in floor heating water circulation system as test sample, and by lacing film.Production of the present invention is not added with another group simultaneously
The service area of product is 100m2Domestic floor system do blank control, the water being added in control group system is identical as experimental group.
After two groups of ground heating systems are run 60 days, stainless steel lacing film is taken out and is cleaned with deionized water, dry weighing, according to sample weight
Amount increases judgement sample surface scale degree.By experiment of weighing data it is found that the gain in weight of blank group lacing film is 0.205g, it is added
The lacing film gain in weight of the inorganic particle scale dispersing agent group provided in the embodiment of the present invention is only 0.03g, sample increase weight quality with
Blank reduces 85% or so.
A specific embodiment of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.
Claims (10)
1. a kind of compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water, which is characterized in that including following raw material: fowler
Alkene, thionyl chloride, diamine, dicyclohexylcarbodiimide, ferric trichloride, anhydrous sodium acetate, hexamethylene diamine.
2. the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 1, which is characterized in that described
Fullerene, thionyl chloride, diamine, dicyclohexylcarbodiimide mass ratio are as follows:
Fullerene: thionyl chloride: diamine: dicyclohexylcarbodiimide=1:3.5~13:0.08~3.2:15~20.
3. the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 2, which is characterized in that described
The molar ratio of anhydrous sodium acetate, ferric trichloride are as follows:
Anhydrous sodium acetate: ferric trichloride=6~9:1；
The mass ratio of the hexamethylene diamine, ferric trichloride are as follows:
Hexamethylene diamine: ferric trichloride=5~7:1；
The molar ratio of the fullerene, ferric trichloride:
Fullerene: ferric trichloride=2~5:1.
4. the preparation of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water described in any one of -3 according to claim 1
Method, which comprises the following steps:
S1, amination modified fullerene；
S2, preparation amination fullerene ferric oxide composite material.
5. the preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 4, special
Sign is, step S1 specifically includes the following steps:
S11, fullerene is taken to be added in sulfuric acid, control reaction temperature is 90 DEG C~120 DEG C, is stirred at reflux, reacts for 6h~12h；
S12, nitric acid is added, control reaction temperature is 70 DEG C~90 DEG C, is stirred at reflux, and the reaction time is 12h~for 24 hours；
S13, it is cooled to room temperature, filters, it is 6.5~7.0 that deionized water, which is washed to pH, is dried in vacuo to obtain acidification fullerene；
S14, acidification fullerene is distributed in solvent dimethylformamide, instills thionyl chloride, is uniformly mixed；
S15, control reaction temperature are 60 DEG C~70 DEG C, are stirred at reflux for 24 hours~36h；
S16, tetrahydrofuran solvent, centrifuge separation is added, vacuum drying obtains chloride fullerene；
S17, chloride fullerene is added in binary amine solvent, dicyclohexylcarbodiimide is added, control reaction temperature is
130 DEG C~160 DEG C, it is stirred at reflux for 24 hours~48h；
S18, dehydrated alcohol, supersound washing is added, filtering is dried in vacuo to obtain amination fullerene.
6. the preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 5, special
Sign is that the mass ratio of fullerene described in step S11 and sulfuric acid is 1:75~137.
7. the preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 5, special
Sign is that the volume ratio of nitric acid described in step S12 and sulfuric acid described in step S11 is 1~1.5:1.
8. the preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 5, special
Sign is that the volume ratio of tetrahydrofuran described in step S16 and thionyl chloride described in step S14 is 20~30:1.
9. the preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 5, special
Sign is that diamine described in step S17 is one or more of ethylenediamine, hexamethylene diamine and decamethylene diamine.
10. the preparation method of the compound scale dispersing agent of the inorganic particle of Domestic floor recirculated water according to claim 4, special
Sign is, step S2 specifically includes the following steps:
S21, take ferric trichloride, anhydrous sodium acetate and hexamethylene diamine be dissolved in in, controlled at 70 DEG C~80 DEG C, stir evenly；
S22, amination fullerene is added, control reaction temperature is 120 DEG C~160 DEG C, reacts 8h~12h, is cooled to room temperature, takes
It filters, is successively cleaned with water and ethyl alcohol out, it is dry；
S23, control heating rate are 3 DEG C/min, and in 150 DEG C~230 DEG C heat preservation sintering 1h~2h, grinding obtains amination fowler
Alkene ferric oxide composite material.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861639A (en) * | 2006-06-08 | 2006-11-15 | 天津大学 | Process of preparing chitosan/carbon nano tube composite material by covalence graft |
| CN105536708A (en) * | 2015-12-28 | 2016-05-04 | 北京林业大学 | Novel composite material based on metal-organic framework material and carbon nanotube and preparation method of novel composite material |
-
2019
- 2019-06-04 CN CN201910482416.4A patent/CN110127864A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861639A (en) * | 2006-06-08 | 2006-11-15 | 天津大学 | Process of preparing chitosan/carbon nano tube composite material by covalence graft |
| CN105536708A (en) * | 2015-12-28 | 2016-05-04 | 北京林业大学 | Novel composite material based on metal-organic framework material and carbon nanotube and preparation method of novel composite material |
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Application publication date: 20190816 |