A block polyether compound, a method for preparing the same, and an application thereof

CN116970159BActive Publication Date: 2026-10-09CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202210427445.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-04-22
Publication Date
2026-10-09
Estimated Expiration
2042-04-22

AI Technical Summary

Technical Problem

[0002]目前油田上使用的清水剂多为溶液型,存在粘度大、操作施工难的问题

Benefits of technology

[0021] The block polyether compound of the present invention has a large molecular weight and good interfacial properties, and has good adsorption performance and obvious oil removal effect.

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Abstract

The present application provides a kind of block polyether compound, its preparation method and application.The molecular formula of the block polyether compound is as shown in formula I), wherein R is wherein n is natural number of 10 or more, m, p and q are independently natural number of 100 or more, and the ratio of the sum of m and q to p is (1.1-1.5):1.
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Description

Technical Field

[0001] This invention provides a block polyether compound. Background Technology

[0002] Currently, most cleaning agents used in oil fields are solution-based, which suffers from high viscosity and difficult operation. Given the current state of use and research of crude oil cleaning agents, as well as increasingly stringent environmental requirements, the research and application of new, high-efficiency cleaning agents is becoming increasingly urgent. Summary of the Invention

[0003] One aspect of the present invention provides a block polyether compound with the molecular formula shown in Formula I).

[0004]

[0005] Where R is

[0006] Where n is a natural number greater than 10, m, p and q are independent natural numbers greater than 100, and the ratio of the sum of m and q to p is (1.1-1.5):1.

[0007] In one specific implementation, the value of n ranges from 10 to 100, and the values ​​of m, p, and q range independently from 100 to 500.

[0008] In one specific embodiment, the weight-average molecular weight of the block polyether compound is between 50,000 and 100,000.

[0009] The second aspect of the present invention provides a method for preparing a block polyether compound as described in the first aspect of the present invention, comprising the following steps:

[0010] 1) Add the catalyst to the initiator, mix and heat to the first temperature, then add ethylene oxide, continue heating to the second temperature, carry out the first reaction in a closed system, stop heating and carry out the second reaction (for example, carry out the second reaction in a closed environment), and then adjust the pressure to negative pressure;

[0011] 2) Heat to a third temperature (e.g., in a closed environment), add propylene oxide, mix, and continue heating to a fourth temperature. Conduct the third reaction in a closed environment. After stopping heating, conduct the fourth reaction. Then adjust the pressure to a negative pressure and simultaneously lower the temperature to ambient temperature to obtain the block polyether compound as described in one of the present invention.

[0012] In one specific embodiment, the catalyst is an inorganic base.

[0013] In one specific embodiment, the inorganic base is potassium hydroxide and / or sodium hydroxide.

[0014] In one specific embodiment, the initiator is dicyandiamide.

[0015] In one specific embodiment, the amount of catalyst is 0.1% to 0.5% and the amount of initiator is 0.5% to 2%, based on the total mass of catalyst, initiator, ethylene oxide and propylene oxide, which is 100% of the total mass.

[0016] In one specific embodiment, the molar ratio of ethylene oxide to propylene oxide is 1:(3-4).

[0017] In one specific embodiment, the first temperature is 115 to 135°C, the second temperature is 125 to 135°C, the third temperature is 125 to 145°C, and the fourth temperature is 140 to 150°C.

[0018] In one specific embodiment, the time for the first reaction and the third reaction is independently defined as the reaction ending when the pressure begins to decrease, and the time for the second reaction and the fourth reaction is independently defined as 25 to 40 minutes.

[0019] The third invention provides the use of the block polyether compound according to the first invention or the block polyether compound prepared by the method according to any one of the second invention as a water-repellent agent or as an effective component of a water-repellent agent.

[0020] The beneficial effects of this invention are:

[0021] The block polyether compound of the present invention has a large molecular weight and good interfacial properties, and has good adsorption performance and obvious oil removal effect. Detailed Implementation

[0022] The present invention will be further described below with reference to the embodiments. However, the embodiments of the present invention are merely illustrative examples and should not be construed as limiting the present invention under any circumstances.

[0023] Example 1

[0024] 1) Using potassium hydroxide, dicyandiamide, ethylene oxide, and propylene oxide as the total materials, with their total mass counted as 100%, add 0.1% of the total material mass of potassium hydroxide to 0.5% of the total material mass of dicyandiamide, stir and heat to 115℃, then add 24.85% of the total material mass of ethylene oxide and continue heating to 125℃. Seal the reaction and stop heating when the pressure in the reaction equipment begins to drop, continue the reaction for 40 minutes; then reduce the pressure in the reaction equipment to negative pressure.

[0025] 2) Reheat to 125℃; then add propylene oxide at a molar ratio of 1:3 for ethylene oxide and propylene oxide, stir and mix evenly, and continue heating to 140℃. Seal the reaction and continue heating until the pressure in the reaction equipment begins to drop. Then stop heating and continue the reaction for 40 minutes. Then reduce the pressure in the reaction equipment to negative pressure and reduce the temperature in the reaction equipment to ambient temperature to obtain product A.

[0026]

[0027] Where R is

[0028] Where n is a natural number greater than 10, m, p and q are independent natural numbers greater than 100, and the ratio of the sum of m and q to p is (1.1-1.5):1.

[0029] The weight-average molecular weight of product A was determined using the ultracentrifugation sedimentation rate method and was 67,000.

[0030] Example 2

[0031] 1) Using potassium hydroxide, dicyandiamide, ethylene oxide, and propylene oxide as the total materials, with their total mass counted as 100%, 0.5% of the total material mass of potassium hydroxide is used as a catalyst. Potassium hydroxide is added to 2% of the total material mass of dicyandiamide resin, stirred, and heated to 135°C. Then, 15.54% of the total material mass of ethylene oxide is added, and the temperature is maintained at 135°C. The reaction is sealed until the pressure in the reaction equipment begins to decrease. Heating is then stopped, and the reaction continues for 25 minutes. Then, the pressure in the reaction equipment is reduced to negative pressure.

[0032] 2) Reheat to 145℃; then add propylene oxide at a molar ratio of 1:4 for ethylene oxide and propylene oxide, stir and mix evenly, and continue to maintain the temperature at 145℃. Seal the reaction and continue heating until the pressure in the reaction equipment begins to drop. Continue the reaction for 25 minutes, then reduce the pressure in the reaction equipment to negative pressure and reduce the temperature in the reaction equipment to ambient temperature to obtain product B.

[0033]

[0034] Where R is

[0035] Where n is a natural number greater than 10, m, p and q are independent natural numbers greater than 100, and the ratio of the sum of m and q to p is (1.1-1.5):1.

[0036] The weight-average molecular weight of product B was determined using the ultracentrifugation sedimentation rate method and was 82,000.

[0037] Example 3

[0038] 1) Using potassium hydroxide, dicyandiamide, ethylene oxide, and propylene oxide as the total materials, with their total mass counted as 100%, 0.3% of the total material mass of potassium hydroxide is used as a catalyst. Potassium hydroxide is added to 1.5% of the total material mass of dicyandiamide resin, stirred, and heated to 120°C. Then, 17.51% of the total material mass of ethylene oxide is added, and the temperature is further increased to 130°C. The reaction is sealed until the pressure in the reaction equipment begins to decrease, at which point heating is stopped, and the reaction continues for 30 minutes. Then, the pressure in the reaction equipment is reduced to negative pressure.

[0039] 2) Reheat to 135℃; then add propylene oxide at a molar ratio of 1:3.5, stir and mix evenly, and continue heating to 150℃. Seal the reaction and continue heating until the pressure in the reaction equipment begins to drop. Stop heating and continue the reaction for 30 minutes. Then reduce the pressure in the reaction equipment to negative pressure and reduce the temperature in the reaction equipment to ambient temperature to obtain product C.

[0040]

[0041] Where R is

[0042] Where n is a natural number greater than 10, m, p and q are independent natural numbers greater than 100, and the ratio of the sum of m and q to p is (1.1-1.5):1.

[0043] The weight-average molecular weight of product C was determined using the ultracentrifugation sedimentation rate method and was 77,000.

[0044] Performance testing

[0045] The products A, B, and C prepared in Examples 1 to 3 were subjected to performance evaluation tests. The test method was as follows: Products A, B, and C were respectively added to oily wastewater with an oil content of 572 mg / L collected from an oilfield, mixed evenly, and then allowed to stand for observation. The concentration of products A, B, and C in the oily wastewater was 240 ppm. The performance evaluation results are shown in Table 1.

[0046] Table 1

[0047] Product A 3min The water was yellowish and contained a lot of flocculent material. 10min The water is clear and has many flocs. Product B 3min The water was yellowish and contained few flocs. 10min The water was yellowish and contained few flocs. Product C 3min The water is clear and has few flocs. 10min The water is clear and has many flocs.

[0048] As shown in the table above, products A, B, and C can all achieve the effect of purifying water, but product C has the fastest reaction speed, rapid water quality changes, and produces less flocs, making it the best.

[0049] While the present invention has been described with reference to specific embodiments, those skilled in the art will understand that various changes can be made without departing from the true spirit and scope of the invention. Furthermore, numerous modifications can be made to the subject, spirit, and scope of the invention to suit specific situations, materials, material compositions, and methods. All such modifications are included within the scope of the claims of the present invention.

Claims

1. A method for preparing a block polyether compound according to the following steps: 1) Add the catalyst to the initiator, mix and heat to the first temperature, then add ethylene oxide, continue heating to the second temperature, conduct the first reaction in a sealed environment, stop heating and proceed to the second reaction, then adjust the pressure to negative pressure; wherein, The initiator is dicyandiamide; 2) Heat to the third temperature, add propylene oxide, mix and continue heating to the fourth temperature, seal and carry out the third reaction, stop heating and carry out the fourth reaction, then adjust the pressure to negative pressure and at the same time reduce the temperature to ambient temperature to obtain the block polyether compound. The total mass of the catalyst, initiator, ethylene oxide, and propylene oxide is 100%, wherein the amount of the catalyst is 0.1% to 0.5%, and the amount of the initiator is 0.5% to 2%. The molar ratio of ethylene oxide to propylene oxide is 1:(3-4). The weight-average molecular weight of the obtained block polyether compound is between 50,000 and 100,000.

2. The method according to claim 1, characterized in that, The catalyst is an inorganic base.

3. The method according to claim 2, characterized in that, The inorganic base is potassium hydroxide and / or sodium hydroxide.

4. The method according to claim 1, characterized in that, The first temperature is 115 to 135°C, the second temperature is 125 to 135°C, the third temperature is 125 to 145°C, and the fourth temperature is 140 to 150°C.

5. The method according to claim 1, characterized in that, The time for the first and third reactions is independently defined as the reaction ending when the pressure begins to decrease, and the time for the second and fourth reactions is independently defined as 25 to 40 minutes.

6. The use of the block polyether compound prepared by the method according to any one of claims 1 to 5 as a water-repellent agent or as an effective component of a water-repellent agent.

Citation Information

Patent Citations

  • Polyether amine and preparation method thereof

    CN103131002A