CN108358965A - A kind of preparation method of diglycolamine dimethylene-phosphonic acid - Google Patents
A kind of preparation method of diglycolamine dimethylene-phosphonic acid Download PDFInfo
- Publication number
- CN108358965A CN108358965A CN201810164219.3A CN201810164219A CN108358965A CN 108358965 A CN108358965 A CN 108358965A CN 201810164219 A CN201810164219 A CN 201810164219A CN 108358965 A CN108358965 A CN 108358965A
- Authority
- CN
- China
- Prior art keywords
- diglycolamine
- dimethylene
- phosphonic acid
- preparation
- finished product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids RP(=O)(OH)2; Thiophosphonic acids, i.e. RP(=X)(XH)2 (X = S, Se)
- C07F9/3804—Phosphonic acids RP(=O)(OH)2; Thiophosphonic acids, i.e. RP(=X)(XH)2 (X = S, Se) not used, see subgroups
- C07F9/3808—Acyclic saturated acids which can have further substituents on alkyl
Abstract
The present invention relates to a kind of preparation method of diglycolamine dimethylene-phosphonic acid, which includes the following steps：（1）Liquid phosphorous acid and hydrochloric acid are added into chemical reaction kettle, then diglycolamine aqueous solution is added dropwise, control temperature is at 40~45 DEG C；（2）Diglycolamine aqueous solution completion of dropwise addition, chemical reaction kettle are warming up to 90~100 DEG C, then the formaldehyde being pumped into advance in high-order dropping tank is added dropwise；（3）Formaldehyde completion of dropwise addition, then heat preservation reflux is concentrated into dense dry, add reverse osmosis water and liquid caustic soda, cooling discharging obtains diglycolamine dimethylene-phosphonic acid semi-finished product；（4）By step（3）Semi-finished product enter press filtration workshop, activated carbon press filtration removal mechanical admixture is added and simultaneously decolourizes, is preferably added water, obtains diglycolamine dimethylene-phosphonic acid finished product.The advantage of the invention is that：Preparation method of the present invention has many advantages, such as that simple for process, reaction condition is mild, production cost is low, good product quality, and the product can effectively inhibit CaCO3Dirt.
Description
Technical field
The present invention relates to organic compound preparation method field, more particularly to a kind of system of diglycolamine dimethylene-phosphonic acid
Preparation Method.
Background technology
With the rapid development of various countries' industrialized production, global shortage of water resources and water pollution getting worse,
Constitute serious worldwide social crisis.China is shortage of water resources and more serious one of the country of damage ratio, is had at present more than 300
A big and medium-sized cities water shortage, wherein 1/3 city serious water shortage, has resulted in serious economic loss and social and environmental problems.In energy
In huge industrial water, cooling water accounts for 50%~80%, so saving cooling water becomes the most important thing of Industrial Water Saving.With following
The continuous improvement of ring cooling water cycles of concentration, incrustation ion（Ca2+、Mg2+）Concentration also increase therewith at multiple, some indissolubles
Salt（CaCO3、CaSO4Deng）Incrustation scale is easily generated on heat exchanger heat transfer surface.Have become control fouling at present using antisludging agent
One of most popular method.Therefore the performance of assessment of scale inhibitor, is rationally of great practical significance using antisludging agent.
Currently, common antisludging agent includes inorganic polyphosphoric acid, organic phosphoric acid, organic phosphine carboxylic acid, acrylic acid and maleic acid
Homopolymer and copolymer.In numerous antisludging agents, organic phosphonic compound not only has excellent scale-inhibiting properties, also has both good
Good corrosion inhibition.Compared with inorganic polyphosphoric acid medicament, organic phospho acid has good chemical stability, not facile hydrolysis, resistance to height
Temperature, dosing is small, good synergistic effect.Organic phospho acid has excellent inhibition CaCO3Dirt, CaSO4The performance of dirt, high agent
There is good corrosion inhibition to metal under the conditions of amount.
The present invention is using diglycolamine, phosphorous acid, hydrochloric acid as primary raw material, using chemical reaction kettle as container, is aided with appropriate
Temperature and reaction time prepare diglycolamine dimethylene-phosphonic acid, have simple production process, of low cost, are arranged without " three wastes "
The advantages of putting.
Invention content
It is sweet with two the technical problem to be solved in the present invention is to provide a kind of preparation method of diglycolamine dimethylene-phosphonic acid
Hydramine, phosphorous acid, hydrochloric acid are that primary raw material is aided with temperature appropriate and reaction time to prepare using chemical reaction kettle as container
Diglycolamine dimethylene-phosphonic acid has simple production process, of low cost, the advantages of discharge without " three wastes ".
In order to solve the above technical problems, the technical scheme is that：A kind of preparation of diglycolamine dimethylene-phosphonic acid
Method, innovative point are：The preparation method includes the following steps：
（1）Liquid phosphorous acid and hydrochloric acid are added into chemical reaction kettle, it is anti-to chemistry that diglycolamine aqueous solution is then slowly added dropwise
Kettle is answered, during dropwise addition, control chemical reaction kettle temperature is at 40~45 DEG C；
（2）After diglycolamine aqueous solution completion of dropwise addition, chemical reaction kettle is to slowly warm up to 90~100 DEG C, is then added dropwise advance
The formaldehyde being pumped into high-order dropping tank；
（3）Formaldehyde completion of dropwise addition, at 100~110 DEG C, heat preservation reflux 4~6 hours, are then concentrated into 120~130 DEG C, add
Reverse osmosis water, cooling discharging obtain diglycolamine dimethylene-phosphonic acid semi-finished product；
（4）By step（3）Diglycolamine dimethylene-phosphonic acid semi-finished product enter press filtration workshop, activated carbon press filtration is added and removes machine
Tool impurity simultaneously decolourizes, and is eventually adding water adjustment content, obtains diglycolamine dimethylene-phosphonic acid finished product.
Further, the step（2）In chemical reaction kettle temperature-rise period, control jacket steam pressure≤0.6MPa
Further, the step（4）The dosage of middle activated carbon, which is diglycolamine dimethylene-phosphonic acid semi-finished product per ton, needs 0.1kg
Activated carbon.
The advantage of the invention is that：The preparation method of diglycolamine dimethylene-phosphonic acid of the present invention, the preparation method have
Simple for process, the advantages that reaction condition is mild, production cost is low, good product quality, and the product can effectively inhibit CaCO3
Dirt.
Specific implementation mode
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment 1
The preparation method of the present embodiment diglycolamine dimethylene-phosphonic acid, the preparation method include the following steps：
（1）2200kg liquid phosphorous acid and 1050kg hydrochloric acid are added into chemical reaction kettle, it is sweet that 1130kg bis- is then slowly added dropwise
Aqueous alkanolamine is to chemical reaction kettle, and during dropwise addition, at 40 DEG C, diglycolamine aqueous solution is added dropwise control chemical reaction kettle temperature
Time is 3 hours；
（2）After diglycolamine aqueous solution completion of dropwise addition, chemical reaction kettle is to slowly warm up to 90 DEG C, and control jacket steam pressure
Then the 2100kg formaldehyde being pumped into advance in high-order dropping tank is added dropwise in≤0.6MPa；
（3）Formaldehyde completion of dropwise addition, at 100 DEG C, heat preservation reflux 6 hours, are then concentrated into 120 DEG C, it is reverse osmosis to add 2000kg
Water, cooling discharging obtain diglycolamine dimethylene-phosphonic acid semi-finished product；
（4）By step（3）Diglycolamine dimethylene-phosphonic acid semi-finished product enter press filtration workshop, activated carbon press filtration is added and removes machine
Tool impurity simultaneously decolourizes, and aminoethyle alcohol dimethylene-phosphonic acid semi-finished product per ton need the activated carbon of 0.1kg, is eventually adding water adjustment and contains
Amount, obtains 7510kg diglycolamine dimethylene-phosphonic acid finished products.
Embodiment 2
The preparation method of the present embodiment diglycolamine dimethylene-phosphonic acid, the preparation method include the following steps：
（1）2200kg liquid phosphorous acid and 1050kg hydrochloric acid are added into chemical reaction kettle, it is sweet that 1130kg bis- is then slowly added dropwise
Aqueous alkanolamine is to chemical reaction kettle, and during dropwise addition, at 45 DEG C, diglycolamine aqueous solution is added dropwise control chemical reaction kettle temperature
Time is 2 hours；
（2）After diglycolamine aqueous solution completion of dropwise addition, chemical reaction kettle is to slowly warm up to 100 DEG C, and control jacket steam pressure
Then the 2100kg formaldehyde being pumped into advance in high-order dropping tank is added dropwise in power≤0.6MPa；
（3）Formaldehyde completion of dropwise addition, at 110 DEG C, heat preservation reflux 4 hours, are then concentrated into 130 DEG C, it is reverse osmosis to add 2000kg
Water, cooling discharging obtain diglycolamine dimethylene-phosphonic acid semi-finished product；
（4）By step（3）Diglycolamine dimethylene-phosphonic acid semi-finished product enter press filtration workshop, activated carbon press filtration is added and removes machine
Tool impurity simultaneously decolourizes, and aminoethyle alcohol dimethylene-phosphonic acid semi-finished product per ton need the activated carbon of 0.1kg, is eventually adding water adjustment and contains
Amount, obtains 7562kg diglycolamine dimethylene-phosphonic acid finished products.
Embodiment 3
The preparation method of the present embodiment diglycolamine dimethylene-phosphonic acid, the preparation method include the following steps：
（1）2200kg liquid phosphorous acid and 1050kg hydrochloric acid are added into chemical reaction kettle, it is sweet that 1130kg bis- is then slowly added dropwise
Aqueous alkanolamine is to chemical reaction kettle, and during dropwise addition, at 43 DEG C, diglycolamine aqueous solution is added dropwise control chemical reaction kettle temperature
Time is 2.5 hours；
（2）After diglycolamine aqueous solution completion of dropwise addition, chemical reaction kettle is to slowly warm up to 95 DEG C, and control jacket steam pressure
Then the 2100kg formaldehyde being pumped into advance in high-order dropping tank is added dropwise in≤0.6MPa；
（3）Formaldehyde completion of dropwise addition, at 105 DEG C, heat preservation reflux 5 hours, are then concentrated into 125 DEG C, it is reverse osmosis to add 2000kg
Water, cooling discharging obtain diglycolamine dimethylene-phosphonic acid semi-finished product；
（4）By step（3）Diglycolamine dimethylene-phosphonic acid semi-finished product enter press filtration workshop, activated carbon press filtration is added and removes machine
Tool impurity simultaneously decolourizes, and aminoethyle alcohol dimethylene-phosphonic acid semi-finished product per ton need the activated carbon of 0.1kg, is eventually adding water adjustment and contains
Amount, obtains 7598k diglycolamine dimethylene-phosphonic acid finished products.
Physical and chemical index by the embodiment 1-3 diglycolamine dimethylene-phosphonic acids prepared is as shown in table 1.
The diglycolamine dimethylene-phosphonic acid prepared by embodiment 1-3 is to CaCO3The application effect of dirt is as shown in table 2.
The physical and chemical index of diglycolamine dimethylene-phosphonic acid prepared by 1 embodiment 1-3 of table
Diglycolamine dimethylene-phosphonic acid prepared by 2 embodiment 1-3 of table is to CaCO3The application effect of dirt
As can be seen from the above table, the result and phenomenon tested from continuous National Standard Method resistance calcium carbonate scale can be seen that diglycolamine two
Methylene phosphonic acid will can be only achieved more satisfactory resistance calcium carbonate scale effect in 20 mg/L or more, but in 4~8mg/L, scale inhibition
Effect is all very poor, i.e., diglycolamine dimethylene-phosphonic acid is very poor in low dosage scale-inhibiting properties, diglycolamine dimethylene
Phosphonic acids can effectively inhibit ground CaCO in high dose3Dirt.
The basic principles and main features and advantages of the present invention of the present invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (3)
1. a kind of preparation method of diglycolamine dimethylene-phosphonic acid, it is characterised in that：The preparation method includes the following steps：
（1）Liquid phosphorous acid and hydrochloric acid are added into chemical reaction kettle, it is anti-to chemistry that diglycolamine aqueous solution is then slowly added dropwise
Kettle is answered, during dropwise addition, control chemical reaction kettle temperature is at 40~45 DEG C；
（2）After diglycolamine aqueous solution completion of dropwise addition, chemical reaction kettle is to slowly warm up to 90~100 DEG C, is then added dropwise advance
The formaldehyde being pumped into high-order dropping tank；
（3）Formaldehyde completion of dropwise addition, at 100~110 DEG C, heat preservation reflux 4~6 hours, are then concentrated into 120~130 DEG C, add
Reverse osmosis water, cooling discharging obtain diglycolamine dimethylene-phosphonic acid semi-finished product；
（4）By step（3）Diglycolamine dimethylene-phosphonic acid semi-finished product enter press filtration workshop, activated carbon press filtration is added and removes machine
Tool impurity simultaneously decolourizes, and is eventually adding water adjustment content, obtains diglycolamine dimethylene-phosphonic acid finished product.
2. the preparation method of diglycolamine dimethylene-phosphonic acid according to claim 1, it is characterised in that：The step
（2）In chemical reaction kettle temperature-rise period, control jacket steam pressure≤0.6MPa.
3. the preparation method of diglycolamine dimethylene-phosphonic acid according to claim 1, it is characterised in that：The step
（4）The dosage of middle activated carbon is the activated carbon that diglycolamine dimethylene-phosphonic acid semi-finished product per ton need 0.1kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810164219.3A CN108358965A (en) | 2018-02-27 | 2018-02-27 | A kind of preparation method of diglycolamine dimethylene-phosphonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810164219.3A CN108358965A (en) | 2018-02-27 | 2018-02-27 | A kind of preparation method of diglycolamine dimethylene-phosphonic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108358965A true CN108358965A (en) | 2018-08-03 |
Family
ID=63003013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810164219.3A Pending CN108358965A (en) | 2018-02-27 | 2018-02-27 | A kind of preparation method of diglycolamine dimethylene-phosphonic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108358965A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4973744A (en) * | 1989-12-15 | 1990-11-27 | W. R. Grace & Co.-Conn. | Ethoxylated N,N-bis-phosphonomethyl 2-(hydroxy)ethylamine N-oxides and water-soluble salts thereof |
| CN101497480A (en) * | 2009-03-02 | 2009-08-05 | 江苏江海化工集团有限公司 | Novel industrial water treatment agent and preparation thereof |
| CN103420505A (en) * | 2012-05-22 | 2013-12-04 | 丁丽 | Preparation method for compound-type diethylene triamine penta(methylene phosphonic acid) scale inhibitor |
| CN106366123A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production process of organic phosphonic acid of recyclable hydrochloric acid wastewater |
-
2018
- 2018-02-27 CN CN201810164219.3A patent/CN108358965A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4973744A (en) * | 1989-12-15 | 1990-11-27 | W. R. Grace & Co.-Conn. | Ethoxylated N,N-bis-phosphonomethyl 2-(hydroxy)ethylamine N-oxides and water-soluble salts thereof |
| CN101497480A (en) * | 2009-03-02 | 2009-08-05 | 江苏江海化工集团有限公司 | Novel industrial water treatment agent and preparation thereof |
| CN103420505A (en) * | 2012-05-22 | 2013-12-04 | 丁丽 | Preparation method for compound-type diethylene triamine penta(methylene phosphonic acid) scale inhibitor |
| CN106366123A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production process of organic phosphonic acid of recyclable hydrochloric acid wastewater |
Non-Patent Citations (1)
| Title |
|---|
| 蒋守红等: ""有机膦酸阻碳酸钙垢性能研究"", 《化学世界》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103508568B (en) | A kind of boiler scale dispersion agent | |
| CN102766158A (en) | Production technology of amino trimethylene phosphonic acid (ATMP) | |
| CN101921022B (en) | Scale and corrosion inhibitor using recycled water as circulating cooling water in fired power plant, method and application thereof | |
| CN102838216A (en) | Corrosion and scale inhibitor for treating water in heating boiler in winter | |
| CN105481116A (en) | Circulating cooling water corrosion and scale inhibitor and preparation method thereof | |
| CN102515373A (en) | Green corrosion and scale inhibitor for hot-water boiler | |
| CN105036360A (en) | Deoxygenating scale inhibitor and preparation method thereof | |
| CN103482655B (en) | Lime-sodium sulfate-carbon dioxide method used for purifying calcium chloride type bittern | |
| CN106630199A (en) | Preparation method of environment-friendly oilfield reinjection water terpolymer scale inhibitor | |
| CN101811783A (en) | Method for preventing long-distance conveyance scale formation of high-concentration wet process phosphoric acid | |
| CN109264876A (en) | Without phosphorus reverse osmosis antisludging agent EDA-PAMAM and preparation method thereof | |
| CN108358965A (en) | A kind of preparation method of diglycolamine dimethylene-phosphonic acid | |
| CN104478104B (en) | A kind of without phosphorus solid anti-scaling compound and using method thereof | |
| CN101955266B (en) | Dimethyl itaconate sulfonate multi-copolymer scale inhibitor and preparation method thereof | |
| CN108148092A (en) | A kind of preparation method of aminoethyle alcohol dimethylene-phosphonic acid | |
| CN102786156A (en) | Sulfonic acid group-containing attapulgite corrosion and scale inhibitor and preparation method as well as application thereof | |
| CN101786733B (en) | Propenol itaconic acid sulfonate multipolymer scale inhibiting agent and preparation method thereof | |
| CN105502695B (en) | A kind of scale cleaning agent and its application method | |
| CN103922491A (en) | Energy-saving scale inhibiting and removing anticorrosion compound medicament for steam boiler and preparation method of medicament | |
| CN102993071A (en) | Method for synthesizing corrosion and scale inhibitor S-carboxyalkylthiosuccinic acid by adopting one-step method | |
| CN101786731B (en) | Ether-based itaconic acid sulfonate type multi-copolymer scale inhibitor and method for preparing same | |
| CN106554854A (en) | A kind of long-acting boiler detergent and preparation method thereof | |
| CN203668036U (en) | Recycling device of multiple-effect evaporation system condensed water for meeting requirement for boiler high-quality water | |
| CN102703250A (en) | Inorganic chemical composition and preparation method thereof | |
| CN105585143A (en) | Scale inhibitor for industrial water treatment and preparation method and application method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180803 |
|
| RJ01 | Rejection of invention patent application after publication |