CN103668250B - A kind of environment-friendly high-efficiency inhibiter and preparation method thereof and application - Google Patents
A kind of environment-friendly high-efficiency inhibiter and preparation method thereof and application Download PDFInfo
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Abstract
The invention discloses a kind of environment-friendly high-efficiency inhibiter and preparation method thereof and application, described environment-friendly high-efficiency inhibiter comprises Folium Bambosae extract 0.1 ~ 2g/L, thiosinamine 0.05 ~ 0.1g/L, tween 0.01 ~ 0.05g/L, quaternary ammonium salt 0.1 ~ 0.2g/L, sodium iodide 0.01 ~ 0.05g/L, and surplus is pickle solution.Described method comprises raw material preparation, preparation steps; The application in steel, aluminium, petrochemical equipment, filtration, pipeline cleaning agent prepared by the described described environment-friendly high-efficiency inhibiter that is applied as.The present invention, based on Folium Bambosae extract and thiosinamine, adds surface active agent tween, quaternary ammonium salt, auxiliary sodium iodide, and the restrainer that surplus pickle solution prepares exists synergistic function.The present invention have nontoxic, cost is low, strong adaptability and obviously inhibit the corrosive nature of acid to metallic substance, steel and aluminium pickling in mineral acid and organic acid can be applicable to, can be applicable to the cleaning of petrochemical equipment, boiler, pipeline, pollution-free, use safety, convenience after inhibiter of the present invention uses.
Description
Technical field
The invention belongs to metal inhibitor technical field, be specifically related to a kind of environment-friendly high-efficiency inhibiter and preparation method thereof and application.
Background technology
Metallic substance occupies very important status in departments such as modern industrial or agricultural, machinery, traffic, transport, national defence and science and technology.Steel has the advantages such as cheap, machining property is good, output is large, is selection, with the metal first considered in material process, is also one of maximum, most widely used metal of current consumption.But metallic substance very easily corrodes, endanger very serious.According to estimates, the iron and steel amount that the whole world is scrapped because of corrosion is every year equivalent to the 1/4-1/3 of annual production; 3.1% ~ 4.5% of national economy total output value (GDP) is accounted for every year by corroding the loss caused.The advantages such as inhibiter is easy to use with it, applied widely, less investment, instant effect, become one of the most effective anticorrosion technique.
In Chemical Manufacture, acid is widely used in pickling, acidleach, acid is stained with and the operations such as oil well acidation.Conventional acid comprises mineral acid and the large class of organic acid two, mineral acid example hydrochloric acid (HCl), sulfuric acid (H
2sO
4), phosphoric acid (H
3pO
4), nitric acid (HNO
3) etc.; Organic acid is as citric acid (C
6h
8o
7), thionamic acid (NH
2sO
3h), oxalic acid (H
2c
2o
4), acetic acid (CH
3cOOH) etc.In practice, inhibiter need be added to suppress the corrosion of hardware in acid solution in every acid treatment process.The eighties in 20th century once developed gratifying inorganic salt inhibiter in the past: chromic salt, nitrite, mercury salt, arsenide, but due to these inorganic salt can carcinogenic and contaminate environment, therefore application is subject to certain restrictions.After entering the eighties in 20th century, people start the research mainly concentrating on organism inhibiter, and what corrosion mitigating effect was desirable has triazole derivative, thiodiphenylamine and derivative, quinoline and its derivates, pyrrole derivative, pyrazole derivatives, thiazole derivative, organic phosphates inhibiter.But the discharge of this kind of organic inhibitor high expensive, and poorly water-soluble, particularly organic phosphates inhibiter can cause water eutrophication, seriously hinders the development and application of inhibiter.The inhibiter of current industrial application is mostly two or more composite organic inhibitor, mainly utilizes the synergistic effect between them to improve corrosion mitigating effect.Compared with single inhibiter, the advantage such as compound corrosion inhibitor has that corrosion mitigating effect is good, stable performance, deficiency between complementary inhibiter; In addition, along with the reinforcement of environmental consciousness, researching and developing out environmentally friendly inhibiter with low cost is domestic and international extensive concern.To sum up, environmentally friendly highly efficiency compositional inhibiter with low cost is researched and developed for jointly paying close attention in the whole world.
Summary of the invention
The first object of the present invention is to provide a kind of environment-friendly high-efficiency inhibiter; Second object is the preparation method providing described environment-friendly high-efficiency inhibiter; 3rd object is the application providing described environment-friendly high-efficiency inhibiter.
The first object of the present invention is achieved in that and comprises Folium Bambosae extract 0.1 ~ 2g/L, thiosinamine 0.05 ~ 0.1g/L, tween 0.01 ~ 0.05g/L, quaternary ammonium salt 0.1 ~ 0.2g/L, sodium iodide 0.01 ~ 0.05g/L, and surplus is pickle solution.
The second object of the present invention is achieved in that and comprises raw material preparation, preparation steps, specifically comprises:
A, raw material prepare: prepare Folium Bambosae extract for subsequent use, and preparation pickle solution, thiosinamine, tween, quaternary ammonium salt, sodium iodide are for subsequent use;
B, preparation: Folium Bambosae extract, thiosinamine, tween, quaternary ammonium salt, sodium iodide are joined stirring and evenly mixing in pickle solution and namely obtain target compound by proportioning raw materials.
The third object of the present invention is achieved in that the application in steel, aluminium, petrochemical equipment, filtration, pipeline cleaning agent prepared by described environment-friendly high-efficiency inhibiter.
The present invention, based on Folium Bambosae extract and thiosinamine, adds surface active agent tween, quaternary ammonium salt, auxiliary sodium iodide, and the restrainer that surplus pickle solution prepares exists synergistic function.The present invention have nontoxic, cost is low, strong adaptability and obviously inhibit the corrosive nature of acid to metallic substance, steel and aluminium pickling in mineral acid and organic acid can be applicable to, can be applicable to the cleaning of petrochemical equipment, boiler, pipeline, pollution-free, use safety, convenience after inhibiter of the present invention uses.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
Environment-friendly high-efficiency inhibiter of the present invention comprises Folium Bambosae extract 0.1 ~ 2g/L, thiosinamine 0.05 ~ 0.1g/L, tween 0.01 ~ 0.05g/L, quaternary ammonium salt 0.1 ~ 0.2g/L, sodium iodide 0.01 ~ 0.05g/L, and surplus is pickle solution.
In described Folium Bambosae extract, Folium Bambusae total flavones content is more than 20%, and outward appearance is brown-red solid.
Described Folium Bambosae extract is that raw material prepares through extracting with the leaf of bamboo.
Described pickle solution is organic acid washing liquor or mineral acid washing lotion.
Described organic acid is one or more in citric acid, thionamic acid, oxalic acid, acetic acid; Described mineral acid is one or more in hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid.
Environment-friendly high-efficiency inhibiter preparation method of the present invention, comprises raw material preparation, preparation steps, specifically comprises:
A, raw material prepare: prepare Folium Bambosae extract for subsequent use, and preparation pickle solution, thiosinamine, tween, quaternary ammonium salt, sodium iodide are for subsequent use;
B, preparation: Folium Bambosae extract, thiosinamine, tween, quaternary ammonium salt, sodium iodide are joined stirring and evenly mixing in pickle solution and namely obtain target compound by proportioning raw materials.
Described Folium Bambosae extract of preparing comprises the following steps:
A, pre-treatment: after the leaf of bamboo gathers, with water rinse removing leaf surfaces dust after removing surface impurity, drain surface-moisture air-dry after be put in convection oven, in 50-70 DEG C of freeze-day with constant temperature 36 ~ 60h, taking-up is pulverized after naturally cooling to room temperature, and particle diameter is the bamboo leaf powder of 300 ~ 400 μm;
B, extraction: bamboo leaf powder is added ethanolic soln 10 ~ 30 DEG C and soak 1 ~ 4h, then at 50-80 DEG C of water-bath refluxing extraction 2 ~ 5h;
C, concentrated: by the ethanol extract suction filtration obtained that refluxes, to remove the leaf of bamboo powder wherein contained, then on a rotary evaporator 40 ~ 80 DEG C solution rotating evaporation concentration to 1/2 ~ 1/3 volume;
D, extraction: the sherwood oil of volume 2 ~ 5 times will be added in the ethanol extract after concentrated, abundant concussion leaves standstill 12-48 hour afterwards, the sherwood oil on upper strata and the extracting solution of lower floor are separated, reclaim upper liquid, lower floor's liquid again to add in separating funnel and adds volume 2 ~ 3 times of sherwood oils, abundant concussion stratification, changed a sherwood oil every 10 ~ 30 minutes, until supernatant liquid is to colourless;
E, aftertreatment: the subnatant after extraction is carried out rotary evaporation, and steam to 40 ~ 60ml, vaporized liquid is put in furnace pot, is placed in air dry oven in 50 ~ 70 DEG C of drying 12 ~ 24h, with the lower solid of crystallization shovel shovel, be target compound Folium Bambosae extract.
Alcohol concn described in step B is 20 ~ 80%, and add-on is solid-to-liquid ratio 1:20 ~ 30.
Suction filtration described in step C is vacuum filtration.
Of the present inventionly be applied as described environment-friendly high-efficiency inhibiter and preparing the application in steel, aluminium, petrochemical equipment, filtration, pipeline cleaning agent.
The preparation method of Folium Bambosae extract of the present invention specifically comprises the following steps:
A. after the leaf of bamboo gathers, with water rinse removing leaf surfaces dust after removing surface impurity, drain large quantity of moisture air-dry after be put in convection oven, in 50-70 DEG C of freeze-day with constant temperature two round the clock, take out after naturally cooling to room temperature and pulverize, particle diameter is about 350 μm;
B. get a certain amount of bamboo leaf powder, add ethanolic soln (volume fraction is 20%-80%) certain volume (solid-liquid ratio is: 1:25) soaking at room temperature 1-4 hour, then refluxing extraction 2-5 hour at water-bath 50-80 DEG C;
C. the ethanol refluxed is carried 2 and gets liquid vacuum filtration, to remove the leaf of bamboo powder wherein contained, then on a rotary evaporator 40-80 DEG C solution rotating is evaporated to certain volume;
D. the liquid rotating after being concentrated by rotary evaporation moves in separating funnel, adds appropriate sherwood oil, fully leaves standstill 12-48 hour after concussion.The sherwood oil on upper strata and the extracting solution of lower floor are separated, reclaim upper liquid, lower floor's liquid again to add in separating funnel and adds appropriate sherwood oil, and fully concussion is static.Changed a sherwood oil every 10-30 minute, until supernatant liquid is to colourless later;
E. the subnatant after extraction is carried out rotary evaporation, steam about 40-60ml, vaporized liquid is put in furnace pot, is placed in air dry oven in 50-70 DEG C until complete drying, then with the lower solid of crystallization shovel shovel, is Folium Bambosae extract.
The present invention overcomes that existing inhibiter is expensive, toxicity is large, the deficiency of contaminate environment, and from wide, the resourceful leaf of bamboo in source, a kind of easy quantification, easily storage are prepared in extraction, easy to use, corrosion mitigating effect good, the Folium Bambosae extract of stable performance coordinates based on thiosinamine, add surface active agent tween, quaternary ammonium salt, auxiliary sodium iodide, there is synergistic function in the restrainer that surplus pickle solution prepares.The present invention have nontoxic, cost is low, strong adaptability and obviously inhibit the corrosive nature of acid to metallic substance, steel and aluminium pickling in mineral acid and organic acid can be applicable to, can be applicable to the cleaning of petrochemical equipment, boiler, pipeline, pollution-free, use safety, convenience after inhibiter of the present invention uses.
The preparation of embodiment 1---Folium Bambosae extract
This leaf of bamboo inhibiter is extracted by the golden leaf of bamboo and is prepared from, wherein:
A. after the golden bamboo leaf of bamboo gathers, with water rinse removing leaf surfaces dust after removing surface impurity, drain large quantity of moisture air-dry after be put in convection oven, in 70oC drying two round the clock, take out after naturally cooling to room temperature and pulverize, particle diameter is about 350 μm;
B. get a certain amount of bamboo leaf powder, add ethanolic soln (volume fraction is 20%-80%) certain volume (solid-liquid ratio is: 1:25) soaking at room temperature 2 hours, then refluxing extraction 1.5 hours under water-bath 80oC;
C. the ethanol extract vacuum filtration will refluxed, to remove the leaf of bamboo powder wherein contained, then evaporates solution rotating with 70 DEG C on a rotary evaporator;
Liquid rotating after rotary evaporation concentrates by d moves in separating funnel, adds appropriate sherwood oil, fully leaves standstill 40 hours after concussion.The sherwood oil on upper strata and the extracting solution of lower floor are separated, reclaim upper liquid, lower floor's liquid again to add in separating funnel and adds appropriate sherwood oil, and fully concussion is static.Changed a sherwood oil every 10 minutes, until supernatant liquid is to colourless later;
E. the subnatant after extraction is carried out rotary evaporation, steam about 60ml, vaporized liquid is put in furnace pot, is placed in air dry oven constant temperature 50 DEG C until complete drying, then with the lower solid of crystallization shovel shovel, is leaf of bamboo inhibiter.
The preparation of embodiment 2---Folium Bambosae extract
This Folium Bambosae extract is extracted by black bamboo leaf and is prepared from, wherein:
A. after the black bamboo leaf of bamboo gathers, with water rinse removing leaf surfaces dust after removing surface impurity, drain large quantity of moisture air-dry after be put in convection oven, round the clock, take out after naturally cooling to room temperature and pulverize, particle diameter is about 350 μm in constant temperature 80oC drying two;
B. get a certain amount of bamboo leaf powder, add ethanolic soln (volume fraction is 20%-80%) certain volume (solid-liquid ratio is: 1:25) soaking at room temperature 1 hour, then refluxing extraction 2 hours at water-bath 60 DEG C;
C. the ethanol extract vacuum filtration will refluxed, to remove the leaf of bamboo powder wherein contained, then evaporates solution rotating with 70 DEG C on a rotary evaporator;
Liquid rotating after rotary evaporation concentrates by d moves in separating funnel, adds appropriate sherwood oil, fully leaves standstill 24 hours after concussion.The sherwood oil on upper strata and the extracting solution of lower floor are separated, reclaim upper liquid, lower floor's liquid again to add in separating funnel and adds appropriate sherwood oil, and fully concussion is static.Changed a sherwood oil every 10 minutes, until supernatant liquid is to colourless later;
E. the subnatant after extraction is carried out rotary evaporation, steam about 40ml, vaporized liquid is put in furnace pot, is placed in air dry oven constant temperature 60 DEG C until complete drying, then with the lower solid of crystallization shovel shovel, is Folium Bambosae extract.
The preparation of embodiment 3---Folium Bambosae extract
This Folium Bambosae extract is extracted by the sweet imperial bamboo leaf of bamboo and is prepared from, wherein:
A. after the sweet imperial bamboo bamboo leaf of bamboo gathers, with water rinse removing leaf surfaces dust after removing surface impurity, drain large quantity of moisture air-dry after be put in convection oven, constant temperature 60oC(± 1oC) dry two round the clock, taking-up is pulverized after naturally cooling to room temperature, and particle diameter is about 350 μm;
B. get a certain amount of bamboo leaf powder, add ethanolic soln (volume fraction is 20%-80%) certain volume (solid-liquid ratio is: 1:25) soaking at room temperature 2 hours, then refluxing extraction 2 hours at water-bath 70 DEG C;
C. the ethanol extract vacuum filtration will refluxed, to remove the leaf of bamboo powder wherein contained, then evaporates solution rotating with 60 DEG C on a rotary evaporator;
Liquid rotating after rotary evaporation concentrates by d moves in separating funnel, adds appropriate sherwood oil, fully leaves standstill 24 hours after concussion.The sherwood oil on upper strata and the extracting solution of lower floor are separated, reclaim upper liquid, lower floor's liquid again to add in separating funnel and adds appropriate sherwood oil, and fully concussion is static.Changed a sherwood oil every 20 minutes, until supernatant liquid is to colourless later;
E. the subnatant after extraction is carried out rotary evaporation, steam about 50ml, vaporized liquid is put in furnace pot, is placed in air dry oven constant temperature 60 DEG C until complete drying, then with the lower solid of crystallization shovel shovel, is Folium Bambosae extract.
Embodiment 4---the preparation of environment-friendly high-efficiency inhibiter
Add the sulfuric acid lotion of concentration 0.5 ~ 5.0mol/L to 1L in Example 1 Folium Bambosae extract 0.1g, thiosinamine 0.05g, tween 0.01g, quaternary ammonium salt 0.1g, sodium iodide 0.01g, obtain target compound environment-friendly high-efficiency inhibiter.
Embodiment 5---the preparation of environment-friendly high-efficiency inhibiter
Add the hydrochloric acid lotion of concentration 1.0 ~ 5.0mol/L to 1L in Example 2 Folium Bambosae extract 2g, thiosinamine 0.1g, tween 0.05g, quaternary ammonium salt 0.2g, sodium iodide 0.05g, obtain target compound environment-friendly high-efficiency inhibiter.
Embodiment 6---the preparation of environment-friendly high-efficiency inhibiter
The hydrochloric acid lotion adding concentration 0.5 – 2.0mol/L in Example 3 Folium Bambosae extract 1g, thiosinamine 0.075g, tween 0.03g, quaternary ammonium salt 0.15g, sodium iodide 0.04g, to 1L, obtains target compound environment-friendly high-efficiency inhibiter.
The pickling of test example 1---ferrous materials
Ferrous materials is chosen as cold rolling steel disc, is injected by composite for embodiment 5 good inhibiter, mixes, and corrosion inhibition all can more than 95% in differing temps (20 ~ 50 DEG C) difference corrosion soak time (2 ~ 148h).Table 1 is 1.0mol/LHCl testing data, and method is weight-loss method.
table 1compound corrosion inhibitor is to the corrosion inhibition rate of cold-rolled steel in HCl
The pickling of test example 2---ferrous materials
Ferrous materials is chosen as cold rolling steel disc, is injected by composite for embodiment 4 good inhibiter, mixes, and corrosion inhibition all can more than 95% in differing temps (20 ~ 60 DEG C) difference corrosion soak time (2 ~ 172h).Table 2 is 1.0mol/LH
2sO
4testing data, method is weight-loss method.
table 2compound corrosion inhibitor to cold-rolled steel at H
2sO
4in corrosion inhibition rate
The pickling of test example 3---commercial-purity aluminium
Metallic substance is chosen as commercial-purity aluminium, is injected by composite for embodiment 6 good inhibiter, mixes, and corrosion inhibition all can more than 90% in differing temps (20 ~ 40 DEG C) difference corrosion soak time (1.0 ~ 3h).Table 3 is 1.0mol/LHCl testing data, and method is weight-loss method.
table 3compound corrosion inhibitor is to the corrosion inhibition rate of commercial-purity aluminium in HCl
Claims (6)
1. an environment-friendly high-efficiency inhibiter, it is characterized in that described environment-friendly high-efficiency inhibiter comprises Folium Bambosae extract 0.1 ~ 2g/L, thiosinamine 0.05 ~ 0.1g/L, tween 0.01 ~ 0.05g/L, quaternary ammonium salt 0.1 ~ 0.2g/L, sodium iodide 0.01 ~ 0.05g/L, surplus is pickle solution; Described Folium Bambosae extract prepares according to the following steps:
A, pre-treatment: after the leaf of bamboo gathers, with water rinse removing leaf surfaces dust after removing surface impurity, drain surface-moisture air-dry after be put in convection oven, in 50 ~ 70 DEG C of freeze-day with constant temperature 36 ~ 60h, taking-up is pulverized after naturally cooling to room temperature, and particle diameter is the bamboo leaf powder of 300 ~ 400 μm;
B, extraction: bamboo leaf powder being added concentration is that 20 ~ 80% ethanolic soln 10 ~ 30 DEG C soaks 1 ~ 4h, and solid-to-liquid ratio 1:20 ~ 30, then at 50 ~ 80 DEG C of water-bath refluxing extraction 2 ~ 5h;
C, concentrated: by the ethanol extract vacuum filtration obtained that refluxes, to remove the leaf of bamboo powder wherein contained, then on a rotary evaporator 40 ~ 80 DEG C solution rotating evaporation concentration to 1/2 ~ 1/3 volume;
D, extraction: the sherwood oil of volume 2 ~ 5 times will be added in the ethanol extract after concentrated, abundant concussion leaves standstill 12 ~ 48 hours afterwards, the sherwood oil on upper strata and the extracting solution of lower floor are separated, reclaim upper liquid, lower floor's liquid again to add in separating funnel and adds volume 2 ~ 3 times of sherwood oils, abundant concussion stratification, changed a sherwood oil every 10 ~ 30 minutes, until supernatant liquid is to colourless;
E, aftertreatment: the subnatant after extraction is carried out rotary evaporation, and steam to 40 ~ 60ml, vaporized liquid is put in furnace pot, is placed in air dry oven in 50 ~ 70 DEG C of drying 12 ~ 24h, with the lower solid of crystallization shovel shovel, be target compound Folium Bambosae extract.
2. environment-friendly high-efficiency inhibiter according to claim 1, it is characterized in that in described Folium Bambosae extract, Folium Bambusae total flavones content is more than 20%, outward appearance is brown-red solid.
3. environment-friendly high-efficiency inhibiter according to claim 1, is characterized in that described pickle solution is organic acid washing liquor or mineral acid washing lotion.
4. environment-friendly high-efficiency inhibiter according to claim 3, is characterized in that described organic acid is one or more in citric acid, thionamic acid, oxalic acid, acetic acid; Described mineral acid is one or more in hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid.
5. the arbitrary described environment-friendly high-efficiency inhibiter preparation method of claim 1 ~ 4, is characterized in that comprising raw material preparation, preparation steps, specifically comprises:
A, raw material prepare: prepare Folium Bambosae extract for subsequent use, and preparation pickle solution, thiosinamine, tween, quaternary ammonium salt, sodium iodide are for subsequent use;
B, preparation: Folium Bambosae extract, thiosinamine, tween, quaternary ammonium salt, sodium iodide are joined stirring and evenly mixing in pickle solution and namely obtain target compound by proportioning raw materials.
6. the application in steel, aluminium, petrochemical equipment, filtration, pipeline cleaning agent prepared by the arbitrary described environment-friendly high-efficiency inhibiter of claim 1 ~ 4.
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| CN105002509B (en) * | 2015-07-30 | 2017-06-30 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method that pickle carries out pickling with corrosion inhibiter and with the pickle with corrosion inhibiter |
| CN104988518B (en) * | 2015-07-30 | 2017-06-30 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of hot rolling acid-cleaning corrosion inhibiter and the method for carrying out pickling with the hot rolling acid-cleaning corrosion inhibiter |
| CN106478879B (en) * | 2015-08-31 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of copolymer and the preparation method and application thereof |
| CN105483713B (en) * | 2015-12-05 | 2017-08-29 | 西南林业大学 | A kind of modified high-molecular compound corrosion inhibitor and preparation method and application |
| CN106978603B (en) * | 2017-04-12 | 2019-06-07 | 西南林业大学 | A kind of plant compound corrosion inhibitor and the preparation method and application thereof |
| CN107142481A (en) * | 2017-06-22 | 2017-09-08 | 西南石油大学 | A kind of method that ginkgo leaf compounding prepares corrosion inhibiter |
| CN107574447B (en) * | 2017-08-09 | 2019-08-02 | 中国石油天然气股份有限公司 | Phosphoric acid restrainer and preparation method thereof |
| CN107557800B (en) * | 2017-09-20 | 2019-12-24 | 旌德君创科技发展有限公司 | Environment-friendly pickling solution applied to aluminum product |
| CN110607529A (en) * | 2019-10-15 | 2019-12-24 | 西南林业大学 | Malignant weed compound corrosion inhibitor and preparation method and application thereof |
| CN110552010A (en) * | 2019-10-15 | 2019-12-10 | 西南林业大学 | Flower plant compound corrosion inhibitor and preparation method and application thereof |
| CN110952101A (en) * | 2019-12-11 | 2020-04-03 | 西南林业大学 | Rubber seed compound corrosion inhibitor and preparation method and application thereof |
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