A method for preparing potassium formate for oilfield chemical additive

Abstract

The invention belongs to the technical field of potassium formate preparation, and discloses a method for preparing potassium formate for oilfield chemical additives. The preparation method comprises the following steps: mixing a catalyst, formaldehyde and a first solvent to obtain a first mixed solution; mixing potassium permanganate and a second solvent to obtain a second mixed solution; mixing the first mixed solution and the second mixed solution, and simultaneously introducing carbon dioxide to react to obtain potassium formate; wherein the catalyst comprises a phase transfer catalyst. The method for preparing potassium formate has mild reaction conditions and low production cost.

Description

Technical Field

[0001] The invention relates to the technical field of potassium formate preparation, in particular to a method for preparing potassium formate for oilfield chemical additives. Background Art

[0002] In the field of oilfield chemical additives, the preparation of potassium formate has always been a research focus. Traditional potassium formate preparation processes often involve complex processes and harsh reaction conditions. For example, some early methods synthesized potassium formate through high temperature and high pressure reactions, which not only consumed a lot of energy to maintain the reaction environment, but also had a long reaction time and low production efficiency. The long reaction process reduced the turnover rate of the equipment and could not meet the growing market demand.

[0003] At present, the preparation method of potassium formate mainly uses potassium hydroxide and formic acid as raw materials. Formic acid is volatile and corrosive. It not only has a certain corrosive effect on equipment and increases equipment maintenance costs, but also has a high price, which makes the production cost high. High energy consumption: After the neutralization reaction, pH adjustment and drying processes are required. Some drying processes require a lot of energy consumption, such as heating and drying, which increases the energy consumption cost of production.

[0004] Therefore, providing a method for preparing potassium formate with mild reaction conditions and low production cost is an urgent problem to be solved. Summary of the invention

[0005] The object of the present invention is to provide a method for preparing potassium formate for oilfield chemical additives, wherein the potassium formate preparation method has mild reaction conditions and low production cost.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The present invention provides a method for preparing potassium formate for oilfield chemical additives, comprising the following steps:

[0008] Mixing the catalyst and the formaldehyde aqueous solution to obtain a first mixed solution;

[0009] Mixing potassium permanganate and water to obtain a second mixed solution;

[0010] The first mixed solution and the second mixed solution are mixed, and carbon dioxide is introduced into the solution to react and obtain potassium formate;

[0011] The catalyst comprises a phase transfer catalyst.

[0012] Preferably, the concentration of formaldehyde in the first mixed solution is 30-40wt%.

[0013] Preferably, the mass of the catalyst is 0.2-3% of the mass of the formaldehyde aqueous solution.

[0014] Preferably, the concentration of potassium permanganate in the second mixed solution is 20-30wt%.

[0015] Preferably, the mass ratio of the first mixed solution to the second mixed solution is 1-3:1-2.

[0016] Preferably, the catalyst comprises at least one of benzyltriethylammonium chloride, tetrabutylammonium bromide, tetrabutylammonium chloride or trioctyltrimethylammonium chloride.

[0017] Preferably, the reaction temperature is 30-60° C., and the reaction time is 20-100 min.

[0018] Preferably, the flow rate of the carbon dioxide is 0.5~5L / min.

[0019] Preferably, after the reaction is completed, post-treatment is also included.

[0020] The post-treatment comprises: separating the product obtained after the reaction to remove the catalyst to obtain a potassium formate solution, and then cooling, crystallizing and drying to obtain potassium formate.

[0021] It can be seen from the above technical solution that compared with the prior art, the present invention has the following beneficial effects:

[0022] The preparation method of potassium formate for oilfield chemical additives provided by the present invention, selects formaldehyde and potassium permanganate as raw materials, and potassium formate is prepared by redox and phase transfer reaction, and the reaction temperature requirement is relatively low, which greatly reduces energy consumption and the high temperature requirement for reaction equipment; the reaction time is short, and production efficiency is effectively improved, and the production cycle is shortened; the cost of raw materials is low, and formaldehyde and potassium permanganate are both common and relatively cheap chemical raw materials, which greatly reduces production costs. More importantly, the method can significantly improve the yield and purity of potassium formate, and provides more favorable conditions for the industrial production of potassium formate. In addition, carbon dioxide is cleverly passed into the reaction process for adjustment, and this measure can significantly reduce the severity of the reaction, so that the reaction temperature is within a controllable range, effectively avoiding the potential safety hazards that may be caused by the reaction being too violent, and further improving the safety and stability of the whole preparation process. DETAILED DESCRIPTION

[0023] The present invention provides a method for preparing potassium formate for oilfield chemical additives, comprising the following steps:

[0024] Mixing the catalyst and the formaldehyde aqueous solution to obtain a first mixed solution;

[0025] Mixing potassium permanganate and water to obtain a second mixed solution;

[0026] The first mixed solution and the second mixed solution are mixed, and carbon dioxide is introduced into the solution to react and obtain potassium formate;

[0027] The catalyst comprises a phase transfer catalyst.

[0028] In the present invention, the concentration of formaldehyde in the first mixed solution is 30-40wt%. As an example, the concentration of formaldehyde in the first mixed solution can be any value of 30wt%, 31wt%, 32wt%, 33wt%, 34wt%, 35wt%, 36wt%, 37wt%, 38wt%, 39wt%, 40wt%, or any value within the range of any two of the above values.

[0029] In the present invention, the mass of the catalyst is 0.2% to 3% of the mass of the formaldehyde aqueous solution. As an example, the mass of the catalyst can be any value of 0.2%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3% of the mass of formaldehyde, or any value within the range of any two of the above values.

[0030] In the present invention, the concentration of potassium permanganate in the second mixed solution is 20-30wt%. As an example, the concentration of potassium permanganate in the second mixed solution can be any value among 20wt%, 21wt%, 22wt%, 23wt%, 24wt%, 25wt%, 26wt%, 27wt%, 28wt%, 29wt%, 30wt% or any value within the range consisting of any two of the above values.

[0031] In the present invention, the mass ratio of the first mixed solution and the second mixed solution is 1~3:1~2. As an example, the volume ratio of the first mixed solution and the second mixed solution can be any value in 1:1, 1:2, 2:1, 3:1 or any value in the range of any two of the above values. By controlling the mass ratio of the first mixed solution and the second mixed solution within the above range, the yield of potassium formate can be improved. If the mass of the first mixed solution is too much and the formaldehyde content is too much, due to the relatively insufficient amount of potassium permanganate, all formaldehyde may not be oxidized to potassium formate, resulting in part of the formaldehyde not reacting or other side reactions; if the mass of the first mixed solution is too little and the formaldehyde content is too little, the excess potassium permanganate may cause an increase in side reactions and generate some other oxidation products, such as potassium carbonate, etc., which will reduce the selectivity of potassium formate, and the yield will not be significantly improved or may even decrease, and the cost and difficulty of subsequent separation and purification will also increase.

[0032] In the present invention, the catalyst includes at least one of benzyltriethylammonium chloride, tetrabutylammonium bromide, tetrabutylammonium chloride or trioctyltrimethylammonium chloride.

[0033] In the present invention, the reaction temperature is 30-60°C, and the reaction time is 20-100 min. As an example, the reaction temperature can be any value of 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, or any value within the range of any two of the above values, and the reaction time can be any value of 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, or any value within the range of any two of the above values.

[0034] In the present invention, the flow rate of the carbon dioxide is 0.5 to 5 L / min. As an example, the flow rate of the carbon dioxide can be any value among 0.5 L / min, 1 L / min, 1.5 L / min, 2 L / min, 2.5 L / min, 3 L / min, 3.5 L / min, 4 L / min, 4.5 L / min, 5 L / min, or any value within the range formed by any two of the above values.

[0035] In the present invention, after the reaction is completed, post-treatment is also included.

[0036] The post-treatment comprises: separating the product obtained after the reaction to remove the catalyst to obtain a solution, and then cooling, crystallizing and drying to obtain potassium formate.

[0037] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0038] Embodiment 1, a method for preparing potassium formate for oilfield chemical additives, comprising the following steps:

[0039] Adding 5 g of benzyltriethylammonium chloride to 500 g of a 37 wt % formaldehyde aqueous solution to obtain a first mixed solution;

[0040] 250 g of a second mixed solution with a concentration of 25 wt % was prepared; 250 g of the second mixed solution was added to 500 g of the first mixed solution, and carbon dioxide was introduced at a flow rate of 2 L / min, and the reaction was carried out at 60° C. for 80 min; after the reaction was completed, the obtained product was filtered, the filtrate was cooled and crystallized, and the obtained product was dried to obtain potassium formate for oilfield chemical additives.

[0041] After testing, the yield of potassium formate for oilfield chemical additives in Example 1 was 95.2% and the purity was 98.5%.

[0042] Embodiment 2, a method for preparing potassium formate for oilfield chemical additives, comprising the following steps:

[0043] Adding 10 g of tetrabutylammonium bromide to 500 g of a 37 wt % formaldehyde aqueous solution to obtain a first mixed solution;

[0044] 500 g of a second mixed solution with a concentration of 30 wt % is prepared; 500 g of the second mixed solution is added to 500 g of the first mixed solution, and carbon dioxide is introduced at a flow rate of 4 L / min, and the reaction is carried out at 40° C. for 60 min; after the reaction is completed, the obtained product is filtered, the filtrate is cooled and crystallized, and the obtained product is dried to obtain potassium formate for oilfield chemical additives.

[0045] After testing, the yield of potassium formate for oilfield chemical additives in Example 2 was 94.8% and the purity was 97.8%.

[0046] Embodiment 3, a method for preparing potassium formate for oilfield chemical additives, comprising the following steps:

[0047] Adding 8 g of benzyltriethylammonium chloride to 500 g of a 37 wt % formaldehyde aqueous solution to obtain a first mixed solution;

[0048] 250 g of a second mixed solution with a concentration of 20 wt % was prepared; 250 g of the second mixed solution was added to 500 g of the first mixed solution, and carbon dioxide was introduced at a flow rate of 1 L / min, and the reaction was carried out at 40° C. for 50 min; after the reaction was completed, the obtained product was filtered, the filtrate was cooled and crystallized, and the obtained product was dried to obtain potassium formate for oilfield chemical additives.

[0049] After testing, the yield of potassium formate for oilfield chemical additives in Example 3 was 95.8% and the purity was 98.4%.

[0050] Embodiment 4, a method for preparing potassium formate for oilfield chemical additives, comprising the following steps:

[0051] Adding 5 g of benzyltriethylammonium chloride to 500 g of a 37 wt % formaldehyde aqueous solution to obtain a first mixed solution;

[0052] 250 g of a second mixed solution with a concentration of 30 wt % was prepared; 250 g of the second mixed solution was added to 500 g of the first mixed solution, and carbon dioxide was introduced at a flow rate of 2 L / min, and the reaction was carried out at 40° C. for 80 min; after the reaction was completed, the obtained product was filtered, the filtrate was cooled and crystallized, and the obtained product was dried to obtain potassium formate for oilfield chemical additives.

[0053] After testing, the yield of potassium formate for oilfield chemical additives in Example 4 was 93.2% and the purity was 99.5%.

[0054] Embodiment 5, a method for preparing potassium formate for oilfield chemical additives, comprising the following steps:

[0055] Adding 13 g of benzyltriethylammonium chloride to 500 g of a 37 wt % formaldehyde aqueous solution to obtain a first mixed solution;

[0056] 300 g of a second mixed solution with a concentration of 22 wt % was prepared; 300 g of the second mixed solution was added to 500 g of the first mixed solution, and carbon dioxide was introduced at a flow rate of 3 L / min, and the reaction was carried out at 40° C. for 80 min; after the reaction was completed, the obtained product was filtered, the filtrate was cooled and crystallized, and the obtained product was dried to obtain potassium formate for oilfield chemical additives.

[0057] After testing, the yield of potassium formate for oilfield chemical additives in Example 5 was 94.9% and the purity was 99.5%.

[0058] Example 6, a method for preparing potassium formate for oilfield chemical additives, is similar to that in Example 1, except that the mass of the formaldehyde aqueous solution is 250 g.

[0059] After testing, the yield of potassium formate for oilfield chemical additives in Example 6 was 95.0% and the purity was 98.0%.

[0060] Comparative Example 1

[0061] A method for preparing potassium formate for oilfield chemical additive is similar to that in Example 1, except that no catalyst is added.

[0062] After testing, the yield of potassium formate for oilfield chemical additives in Comparative Example 1 was 85.3% and the purity was 90.3%.

[0063] Comparative Example 2

[0064] A method for preparing potassium formate for oilfield chemical additive is similar to that in Example 1, except that no carbon dioxide is introduced.

[0065] After testing, the yield of potassium formate for oilfield chemical additives in Comparative Example 2 was 87.3% and the purity was 89.8%.

[0066] It can be seen from the test data of the embodiment and the comparative example that the yield and purity of potassium formate prepared in the embodiment are higher than those in the comparative example, indicating that potassium formate is prepared by oxidation-reduction and phase transfer reaction using formaldehyde and potassium permanganate as raw materials, and the introduction of carbon dioxide during the reaction process can greatly improve the yield and purity of the product potassium formate.

[0067] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing potassium formate for oilfield chemical additives, characterized in that: The following steps are involved: Mixing the catalyst and the formaldehyde aqueous solution to obtain a first mixed solution; Mixing potassium permanganate and water to obtain a second mixed solution; The first mixed solution and the second mixed solution are mixed, and carbon dioxide is introduced into the solution to react and obtain potassium formate; The catalyst is a phase transfer catalyst.

2. The method for preparing potassium formate for oilfield chemical additives according to claim 1, characterized in that: The concentration of formaldehyde in the first mixed solution is 30-40wt%; And / or, the mass of the catalyst is 0.2-3% of the mass of the formaldehyde aqueous solution.

3. The method for preparing potassium formate for oilfield chemical additive according to claim 1, characterized in that: The concentration of potassium permanganate in the second mixed solution is 20-30wt%.

4. The method for preparing potassium formate for oilfield chemical additives according to claim 1, characterized in that: The mass ratio of the first mixed solution to the second mixed solution is 1-3:1-2.

5. The method for preparing potassium formate for oilfield chemical additive according to claim 1, characterized in that: The catalyst includes at least one of benzyltriethylammonium chloride, tetrabutylammonium bromide or tetrabutylammonium chloride.

6. The method for preparing potassium formate for oilfield chemical additive according to claim 1, characterized in that: The reaction temperature is 30-60° C., and the reaction time is 20-100 min.

7. The method for preparing potassium formate for oilfield chemical additive according to claim 1, characterized in that: The flow rate of the carbon dioxide is 0.5~5L / min.

8. The method for preparing potassium formate for oilfield chemical additive according to claim 1, characterized in that: After the reaction is completed, post-treatment is also included. The post-treatment comprises: separating the product obtained after the reaction to remove the catalyst to obtain a solution, and then cooling, crystallizing and drying to obtain potassium formate.