CN114057283A - Light nitrogen and phosphorus removal filler utilizing pyrite to modify waste polyurethane and preparation method thereof - Google Patents
Light nitrogen and phosphorus removal filler utilizing pyrite to modify waste polyurethane and preparation method thereof Download PDFInfo
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- CN114057283A CN114057283A CN202111392157.XA CN202111392157A CN114057283A CN 114057283 A CN114057283 A CN 114057283A CN 202111392157 A CN202111392157 A CN 202111392157A CN 114057283 A CN114057283 A CN 114057283A
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- soft foam
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F2003/001—Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms
Abstract
The invention discloses a lightweight nitrogen and phosphorus removal filler utilizing pyrite to modify waste polyurethane and a preparation method thereof, belonging to the field of environmental protection. The method comprises the steps of crushing recovered waste soft foam polyurethane, mixing the crushed waste soft foam polyurethane with soft foam polyether polyol, mixing the crushed waste soft foam polyurethane with an activity regulator and a processing modifier to obtain a primary filler, uniformly mixing the primary filler with natural pyrite powder and sulfur powder, carrying out high-temperature melting granulation, carrying out extrusion molding, and cooling to obtain the product. The method is applied to a synchronous nitrogen and phosphorus removal process, the waste polyurethane recovery product is modified into the light synchronous nitrogen and phosphorus removal filler through natural pyrite powder, and the light synchronous nitrogen and phosphorus removal filler is applied to a fluidized bed reactor, so that the application range and the nitrogen and phosphorus removal efficiency of the pyrite product are greatly improved.
Description
Technical Field
The invention relates to the field of environmental protection, and in particular relates to a lightweight nitrogen and phosphorus removal filler utilizing pyrite to modify waste polyurethane and a preparation method thereof.
Background
In recent years, polyurethane products have been increasingly favored and widely used. Although polyurethane has been labeled with environmentally friendly, recyclable labels, it is not desirable to recycle polyurethane materials after they are actually made into end products. The factories producing polyurethane foams generate a large amount of scrap, mold flash, and waste products each year, and also generate a large amount of waste products such as old polyurethane foams and elastomers in scrapped cars in various downstream application fields, which are required to be recycled. How to recycle waste polyurethane products becomes a research hotspot.
At present, polyurethane is recovered and then is treated by burning, landfill and other modes. The landfill method occupies land and has high consumption. The polyurethane is a nitrogenous polymer, so that the combustion conditions must be strictly controlled to avoid the pollution of toxic and harmful gases to the environment, and the treatment cost is high.
Disclosure of Invention
Aiming at the existing technical problems, the invention provides a light nitrogen and phosphorus removal filler utilizing pyrite to modify waste polyurethane and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of light nitrogen and phosphorus removal filler by utilizing pyrite to modify waste polyurethane comprises the following steps:
step 1: performing surface cleaning treatment on the recovered waste soft foam polyurethane, and then crushing and grinding at low temperature to prepare fine particles with the particle size of 0.1-5 mm; adding the pre-ground fine particles into the soft foam polyether polyol, and wet-grinding the mixture into a fine particle mixture by using a grinding machine;
step 2: adding an activity regulator and a processing modifier into the fine particle mixture prepared in the step 1, cooling to 20-30 ℃, and curing to obtain a primary filler;
and step 3: and (3) uniformly mixing the primary filler obtained in the step (2) with natural pyrite powder and sulfur powder, carrying out high-temperature melting granulation, carrying out extrusion molding, and cooling to obtain the product.
In some preferred embodiments: the particle size of the fine particles was 1 mm.
The preparation method comprises the following steps: 45-70 parts of waste soft foam polyurethane, 6-20 parts of soft foam polyether polyol, 2-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 8-20 parts of natural pyrite powder and 10-30 parts of sulfur powder.
Preferably: 50-60 parts of waste soft foam polyurethane, 10-15 parts of soft foam polyether polyol, 5-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 10-20 parts of natural pyrite powder and 10-30 parts of sulfur powder.
The preparation method comprises the following steps: the activity regulator is a compound containing inorganic active factors selected from Fe2+、Fe3+、Ca2+Or Zn2+One or more of (a).
Preferably, the method comprises the following steps: the activity regulator is prepared from the following components in a mass ratio of 1-3: 1-3: 1-3 FeCl3、MgCl2And FeCl2(ii) a Or the activity regulator is prepared from the following components in a mass ratio of 1-3: 1-3 FeCl3And CaCl2。
The preparation method comprises the following steps: the processing modifier is stearic acid and/or stearate as the preferable: the processing modifier is prepared from the following raw materials in a mass ratio of 1-3: 1 to 3 of stearic acid and a stearate
The preparation method comprises the following steps: the particle size of the pyrite powder is 200-80 meshes, and the particle size of the sulfur powder is 200-80 meshes.
The preparation method comprises the following steps: the high-temperature melting is carried out at 100-200 ℃.
A lightweight nitrogen and phosphorus removal filler utilizing pyrite to modify waste polyurethane is prepared by the following steps:
step 1: carrying out surface cleaning treatment on the recovered waste soft foam polyurethane, and then, carrying out low-temperature crushing and grinding processes to obtain fine particles with the particle size of 1 mm; adding the pre-ground fine particles into the soft foam polyether polyol, and wet-grinding the mixture into a fine particle mixture by using a grinding machine;
step 2: adding an activity regulator and a processing modifier into the fine particle mixture prepared in the step one, cooling to 20-30 ℃, and curing to obtain a primary filler;
and step 3: and D, uniformly mixing the primary filler in the step two with natural pyrite powder and sulfur powder, carrying out high-temperature melting granulation, carrying out extrusion molding, and cooling to obtain the product.
The light denitrification and dephosphorization filler comprises: 45-70 parts of waste soft foam polyurethane, 6-20 parts of soft foam polyether polyol, 2-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 8-20 parts of natural pyrite powder and 10-30 parts of sulfur powder.
Preferably: 50-60 parts of waste soft foam polyurethane, 10-15 parts of soft foam polyether polyol, 5-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 10-20 parts of natural pyrite powder and 10-30 parts of sulfur powder.
The light denitrification and dephosphorization filler comprises: the activity regulator is a compound containing inorganic active factors selected from Fe2+、Fe3+、Ca2+Or Zn2+One or more of;
the light denitrification and dephosphorization filler comprises: the particle size of the pyrite powder is 200-80 meshes, and the particle size of the sulfur powder is 200-80 meshes.
The light denitrification and dephosphorization filler comprises: the high-temperature melting is carried out at 100-200 ℃.
The invention has the beneficial effects that:
the method is applied to a synchronous nitrogen and phosphorus removal process, the waste polyurethane recovery product is modified into the light synchronous nitrogen and phosphorus removal filler through natural pyrite powder, and the light synchronous nitrogen and phosphorus removal filler is applied to a fluidized bed reactor, so that the application range and the nitrogen and phosphorus removal efficiency of the pyrite product are greatly improved. The invention has good development and application prospects in the field of sewage treatment, especially in the aspect of upgrading advanced treatment of town tail water. Compared with natural nitrogen and phosphorus removal filler, the filler has the advantages of small specific gravity, convenient engineering filling and high porosity, greatly increases microorganism attachment and reaction points, and improves the reaction efficiency of nitrogen and phosphorus removal.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
example 1
Step one, the recovered waste soft foam polyurethane (60g) is subjected to surface cleaning treatment, and then is subjected to low-temperature crushing and grinding processes to obtain fine particles with the particle size of 1 mm. Adding the pre-ground fine particles into soft foam polyether polyol (10g), and wet-grinding into a fine particle mixture by using a grinding machine;
step two will be mixed with an activity modifier (FeCl)32g、MgCl22g、FeCl21g of the mixture), and a processing modifier (0.3g, the components are a mixture of 0.15g of sodium stearate and 0.15g of stearic acid), are added into the fine particle mixture prepared in the first step, the temperature is reduced to 20 ℃, and after solidification, a primary filler is obtained;
step three, uniformly mixing the primary filler in the step two with natural pyrite powder (10g) and sulfur powder (10g), carrying out high-temperature melting granulation (140 ℃), carrying out extrusion molding to prepare 3mm granules, and cooling for 2 minutes to obtain the product.
The prepared light polyurethane filler is used for advanced treatment of municipal tail water with low carbon-nitrogen ratio, and meets the requirements of dephosphorization and denitrification for upgrading. Light filler NO3The N removal rate was 91.91% and the TN removal rate was 89.93%. The quality of tail water of a sewage plant is as follows: COD 38mg/L, NO3N11 mg/L and TN 14mg/L, and the tail water of the sewage plant is taken as a treatment object; the effluent quality is as follows: COD 35mg/L, NO3-N 0.89mg/L，TN 1.41mg/L。
Example 2
Step one, the recovered waste soft foam polyurethane (56g) is subjected to surface cleaning treatment, and then is subjected to low-temperature crushing and grinding processes to obtain fine particles with the particle size of 1 mm. Adding the pre-ground fine particles into soft foam polyether polyol (13g), and wet-grinding into a fine particle mixture by using a grinding mill;
step two, mixing the active regulator (the component is FeCl)32g、MgCl23g、CaCl22g of the mixture), and a processing modifier (0.25 g of sodium stearate and 0.25g of stearic acid) are added into the fine particle mixture prepared in the step one, the temperature is reduced to 25 ℃, and after solidification, a primary filler is obtained;
step three, uniformly mixing the primary filler obtained in the step two with natural pyrite powder (13g) and sulfur powder (20g), carrying out high-temperature melting granulation (150 ℃), carrying out extrusion molding to prepare 5mm granules, and cooling for 3 minutes to obtain the product.
The prepared light polyurethane filler is used for emergency treatment engineering of riverways, and the water quality of riverway water is improved. Light filler NO3The N removal rate was 90.27%, and the TN removal rate was 87.68%. River water quality before treatment: COD 20mg/L, NO3-N7.4 mg/L, TN 8.2 mg/L; the effluent quality is as follows: COD 15mg/L, NO3-N 0.72mg/L，TN 1.01mg/L。
Example 3
Step one, the recovered waste soft foam polyurethane (50g) is subjected to surface cleaning treatment, and then is subjected to low-temperature crushing and grinding processes to obtain fine particles with the particle size of 1 mm. Adding the pre-ground fine particles into soft foam polyether polyol (11g), and wet-grinding into a fine particle mixture by using a grinding mill;
step two will be mixed with an activity modifier (FeCl)35g、CaCl25g) Adding a processing modifier (0.5g of sodium stearate and 0.5g of stearic acid) into the fine particle mixture prepared in the step one, cooling to 25 ℃, and curing to obtain a primary filler;
step three, uniformly mixing the primary filler in the step two with natural pyrite powder (16g) and sulfur powder (25g), carrying out high-temperature melting granulation (160 ℃), carrying out extrusion molding to prepare 4mm granules, and cooling for 5 minutes to obtain the product.
The prepared light polyurethane filler is used for sewage of a certain chemical industrial park to carry out nitrogen and phosphorus upgrading. Light filler NO3The N removal rate is 85.96 percent, and the TN removal rate is 82.36 percent; the influent water quality COD is 60mg/L，NO3-N26 mg/L, TN 33 mg/L; the effluent quality is as follows: COD 50mg/L, NO3-N 3.65mg/L，TN 5.82mg/L。
Comparative example 1
The sewage of a certain chemical industry park in the example 3 is treated as raw water by taking the existing commercial polyurethane filler as a treatment medium. The influent water quality COD is 60mg/L and NO3-N26 mg/L, TN 33 mg/L; the effluent quality is as follows: COD 57mg/L, NO3-N15.30 mg/L, TN 21.14 mg/L. Currently commercially available polyurethane fillers NO3The N removal rate was 41.15% and the TN removal rate was 35.94%.
Claims (10)
1. A preparation method of light nitrogen and phosphorus removal filler by using pyrite modified waste polyurethane is characterized by comprising the following steps: the method comprises the following steps:
step 1: performing surface cleaning treatment on the recovered waste soft foam polyurethane, and then crushing and grinding at low temperature to prepare fine particles with the particle size of 0.1-5 mm; adding the fine particles into the soft foam polyether polyol, and wet-milling the fine particles into a fine particle mixture by using a mill;
step 2: adding an activity regulator and a processing modifier into the fine particle mixture prepared in the step 1, cooling to 20-30 ℃, and curing to obtain a primary filler;
and step 3: and (3) uniformly mixing the primary filler obtained in the step (2) with natural pyrite powder and sulfur powder, carrying out high-temperature melting granulation, carrying out extrusion molding, and cooling to obtain the product.
2. The method of claim 1, wherein: 45-70 parts of waste soft foam polyurethane, 6-20 parts of soft foam polyether polyol, 2-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 8-20 parts of natural pyrite powder and 10-30 parts of sulfur powder;
preferably: 50-60 parts of waste soft foam polyurethane, 10-15 parts of soft foam polyether polyol, 5-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 10-20 parts of natural pyrite powder and 10-30 parts of sulfur powder.
3. The method of claim 2, wherein: the activity regulator is a compound containing inorganic active factors selected from Fe2+、Fe3+、Ca2+Or Zn2+One or more of; the activity regulator is prepared from the following components in a mass ratio of 1-3: 1-3: 1-3 FeCl3、MgCl2And FeCl2(ii) a Or the activity regulator is prepared from the following components in a mass ratio of 1-3: 1-3 FeCl3And CaCl2。
4. The method of claim 2, wherein: the processing modifier is stearic acid and/or stearate.
5. The method of claim 4, wherein: the processing modifier is prepared from the following raw materials in a mass ratio of 1-3: 1 to 3 of stearic acid and a stearate.
6. The method of claim 1, wherein: the temperature of the high-temperature melting is 100-200 ℃.
7. A lightweight nitrogen and phosphorus removal filler utilizing pyrite to modify waste polyurethane is characterized in that: the filler is prepared by the following steps:
step 1: carrying out surface cleaning treatment on the recovered waste soft foam polyurethane, and then, carrying out low-temperature crushing and grinding processes to obtain fine particles with the particle size of 1 mm; adding the pre-ground fine particles into the soft foam polyether polyol, and wet-grinding the mixture into a fine particle mixture by using a grinding machine;
step 2: adding an activity regulator and a processing modifier into the fine particle mixture prepared in the step one, cooling to 20-30 ℃, and curing to obtain a primary filler;
and step 3: and D, uniformly mixing the primary filler in the step two with natural pyrite powder and sulfur powder, carrying out high-temperature melting granulation, carrying out extrusion molding, and cooling to obtain the product.
8. The lightweight nitrogen and phosphorus removal filler according to claim 7, wherein: 45-70 parts of waste soft foam polyurethane, 6-20 parts of soft foam polyether polyol, 2-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 8-20 parts of natural pyrite powder and 10-30 parts of sulfur powder;
preferably: 50-60 parts of waste soft foam polyurethane, 10-15 parts of soft foam polyether polyol, 5-10 parts of activity regulator, 0.3-1.5 parts of processing modifier, 10-20 parts of natural pyrite powder and 10-30 parts of sulfur powder.
9. The lightweight nitrogen and phosphorus removal filler according to claim 7, wherein: the activity regulator is a compound containing inorganic active factors selected from Fe2+、Fe3+、Ca2+Or Zn2+One or more of;
the processing modifier is stearic acid and/or stearate; preferably: the processing modifier is prepared from the following raw materials in a mass ratio of 1-3: 1 to 3 of stearic acid and a stearate.
10. The lightweight nitrogen and phosphorus removal filler according to claim 7, wherein: the temperature of the high-temperature melting is 100-200 ℃.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326559A (en) * | 2014-10-08 | 2015-02-04 | 环境保护部南京环境科学研究所 | System for strengthening post-denitrification denitrogenation process |
| CN105399202A (en) * | 2015-12-29 | 2016-03-16 | 北京工业大学 | Method for removing phosphorous based on high-efficiency promotion of spongy iron corrosion in process of nitrogen removal by denitrification |
| CN105836881A (en) * | 2016-06-04 | 2016-08-10 | 北京工业大学 | Reclaimed water deep denitrification and dephosphorization method based on low C/N ratio |
| CN109879419A (en) * | 2019-03-06 | 2019-06-14 | 苏州方舟环保科技有限公司 | The filler special and preparation method thereof of sulphur iron coupling technique removal nitrate nitrogen |
| CN109912963A (en) * | 2019-03-23 | 2019-06-21 | 天津市海纳源科技有限公司 | A kind of production method of waste old powder filled polyurethane plastics |
| CN110002610A (en) * | 2019-04-23 | 2019-07-12 | 南京大学 | A kind of siderite modified sulfur light material and the preparation method and application thereof |
| CN110078221A (en) * | 2019-04-23 | 2019-08-02 | 南京大学 | A kind of synchronous denitrification dephosphorizing light material and its preparation and application method |
| CN110683631A (en) * | 2019-08-21 | 2020-01-14 | 南京华创环境技术研究院有限公司 | Synchronous nitrogen and phosphorus removal composite filler and preparation method and application thereof |
| CN112499759A (en) * | 2020-12-10 | 2021-03-16 | 泉州南京大学环保产业研究院 | Nitrogen and phosphorus removal foaming filler and preparation method thereof |
| CN112723523A (en) * | 2020-12-03 | 2021-04-30 | 南京华创环境技术研究院有限公司 | Carbon-source-free synchronous nitrogen and phosphorus removal filler based on composite sulfur component, and preparation method and application thereof |
-
2021
- 2021-11-23 CN CN202111392157.XA patent/CN114057283A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326559A (en) * | 2014-10-08 | 2015-02-04 | 环境保护部南京环境科学研究所 | System for strengthening post-denitrification denitrogenation process |
| CN105399202A (en) * | 2015-12-29 | 2016-03-16 | 北京工业大学 | Method for removing phosphorous based on high-efficiency promotion of spongy iron corrosion in process of nitrogen removal by denitrification |
| CN105836881A (en) * | 2016-06-04 | 2016-08-10 | 北京工业大学 | Reclaimed water deep denitrification and dephosphorization method based on low C/N ratio |
| CN109879419A (en) * | 2019-03-06 | 2019-06-14 | 苏州方舟环保科技有限公司 | The filler special and preparation method thereof of sulphur iron coupling technique removal nitrate nitrogen |
| CN109912963A (en) * | 2019-03-23 | 2019-06-21 | 天津市海纳源科技有限公司 | A kind of production method of waste old powder filled polyurethane plastics |
| CN110002610A (en) * | 2019-04-23 | 2019-07-12 | 南京大学 | A kind of siderite modified sulfur light material and the preparation method and application thereof |
| CN110078221A (en) * | 2019-04-23 | 2019-08-02 | 南京大学 | A kind of synchronous denitrification dephosphorizing light material and its preparation and application method |
| US20200338485A1 (en) * | 2019-04-23 | 2020-10-29 | Nanjing University | Method for preparing simultaneous nitrogen and phosphorus removal lightweight material and the use thereof |
| CN110683631A (en) * | 2019-08-21 | 2020-01-14 | 南京华创环境技术研究院有限公司 | Synchronous nitrogen and phosphorus removal composite filler and preparation method and application thereof |
| CN112723523A (en) * | 2020-12-03 | 2021-04-30 | 南京华创环境技术研究院有限公司 | Carbon-source-free synchronous nitrogen and phosphorus removal filler based on composite sulfur component, and preparation method and application thereof |
| CN112499759A (en) * | 2020-12-10 | 2021-03-16 | 泉州南京大学环保产业研究院 | Nitrogen and phosphorus removal foaming filler and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 周彦卿;郝瑞霞;刘思远;王丽沙;: "新型硫铁复合填料强化再生水深度脱氮除磷", 环境科学, no. 10, pages 325 - 331 * |
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